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16940-66-2

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16940-66-2 Usage

Check Digit Verification of cas no

The CAS Registry Mumber 16940-66-2 includes 8 digits separated into 3 groups by hyphens. The first part of the number,starting from the left, has 5 digits, 1,6,9,4 and 0 respectively; the second part has 2 digits, 6 and 6 respectively.
Calculate Digit Verification of CAS Registry Number 16940-66:
(7*1)+(6*6)+(5*9)+(4*4)+(3*0)+(2*6)+(1*6)=122
122 % 10 = 2
So 16940-66-2 is a valid CAS Registry Number.
InChI:InChI=1/C4H5B/c1-2-4-5-3-1/h1-5H

16940-66-2SDS

SAFETY DATA SHEETS

According to Globally Harmonized System of Classification and Labelling of Chemicals (GHS) - Sixth revised edition

Version: 1.0

Creation Date: Aug 12, 2017

Revision Date: Aug 12, 2017

1.Identification

1.1 GHS Product identifier

Product name sodium borohydride

1.2 Other means of identification

Product number -
Other names boron sodium hydride

1.3 Recommended use of the chemical and restrictions on use

Identified uses For industry use only.
Uses advised against no data available

1.4 Supplier's details

1.5 Emergency phone number

Emergency phone number -
Service hours Monday to Friday, 9am-5pm (Standard time zone: UTC/GMT +8 hours).

More Details:16940-66-2 SDS

16940-66-2Synthetic route

Trimethyl borate
121-43-7

Trimethyl borate

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
Heating;99.5%
In neat (no solvent) 1mol B(OCH3)3, 4mol NaH, 225-275°C;; 90-96% NaBH4;;94%
In neat (no solvent) 1mol B(OCH3)3, 4mol NaH, 225-275°C;; 90-96% NaBH4;;94%
boric acid trimethylester tetrahydrofuranate

boric acid trimethylester tetrahydrofuranate

Tetrahydro-furan; compound with trifluoroborane

Tetrahydro-furan; compound with trifluoroborane

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In tetrahydrofuran byproducts: NaF; addn. of B(OCH3)3*THF to NaH at 60-65°C (stirring, N2-atmosphere), NaH dissolves, boiling, cooling to ambient temp., addn. of BF3*THF, distn. of THF and B(OCH3), extractn. of residue with isopropyl amine;; pure product;;99%
In tetrahydrofuran byproducts: NaF; addn. of B(OCH3)3*THF to NaH at 60-65°C (stirring, N2-atmosphere), NaH dissolves, boiling, cooling to ambient temp., addn. of BF3*THF, distn. of THF and B(OCH3), extractn. of residue with isopropyl amine;; pure product;;99%
neodymium borohydride * 3 tetrahydrofuran

neodymium borohydride * 3 tetrahydrofuran

disodium 5,6-dihydro-1,4-dithiine-2,3-dithiolate

disodium 5,6-dihydro-1,4-dithiine-2,3-dithiolate

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

[Na3(tetrahydrofuran)1.5Nd(5,6-dihydro-1,4-dithiine-2,3-dithiolate)3]

[Na3(tetrahydrofuran)1.5Nd(5,6-dihydro-1,4-dithiine-2,3-dithiolate)3]

Conditions
ConditionsYield
In tetrahydrofuran (Ar); a flask charged with Nd complex, THF condensed, C4H4S2(SNa)2 added, stirred for 3 d at 20°C; filtered, evapd., extd. (THF), filtered; obtained impure;A n/a
B 99%
sodium hydride
7646-69-7

sodium hydride

diborane
19287-45-7

diborane

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In further solvent(s) react. of NaH with B2H6 in alkylene glycol dialkylether at 35-75°C;;98%
In tetrahydrofuran in abs. tetrahydrofurane; 4 h, under shaking; good yield; Na(BH4) suspension distilled, filtered and dried in oil pump vacuum at 130°C; purity = 97.5 %;93%
In tetrahydrofuran in abs. tetrahydrofurane; 4 h, under shaking; good yield; Na(BH4) suspension distilled, filtered and dried in oil pump vacuum at 130°C; purity = 97.5 %;93%
N,N,N,N,-tetramethylethylenediamine
110-18-9

N,N,N,N,-tetramethylethylenediamine

NaZn(BH4)3*3DME

NaZn(BH4)3*3DME

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

N,N,N',N'-tetramethylethylenediaminebis(tetrahydroborate)zinc(II)

N,N,N',N'-tetramethylethylenediaminebis(tetrahydroborate)zinc(II)

Conditions
ConditionsYield
In benzene org. compd. soln. addn. dropwise (magnetic stirring) to Zn-complex soln., NaBH4 ppt. filtration off after 1 h, solvent evapn. from filtrate (vac.); residue washing (pentane), drying (vac.); elem. anal; thermal anal.;A 77%
B 97%
trifluoroborane diethyl ether
109-63-7

trifluoroborane diethyl ether

sodium hydride
7646-69-7

sodium hydride

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

diborane
19287-45-7

diborane

Conditions
ConditionsYield
In diethylene glycol method for preparation of diborane, addn. of BF3-etherate (frehly distd.) to NaH in diglyme;;A n/a
B 92%
In diethylene glycol method for preparation of diborane, addn. of BF3-etherate (frehly distd.) to NaH in diglyme;;A n/a
B 92%
In diethyl ether at 110°C, method for preparation of diborane;;
In diethyl ether at 110°C, method for preparation of diborane;;
borax

borax

hydrogen
1333-74-0

hydrogen

sodium hydroxide
1310-73-2

sodium hydroxide

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
magnesium In water byproducts: MgO; process starts from borax and NaOH by exothermal steam process (H2O); dread at 270°C; H2 at surface of Mg particles generated protide to form NaBH4; process dependent on of rate temp. change, size of Mg particles; XRD;90%
boron trifluoride
7637-07-2

boron trifluoride

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
With catalyst: Na-alcoholate In neat (no solvent) passing BF3 over NaH in presence of a Na-alcoholate, 250-300°C;;90%
In neat (no solvent) byproducts: B2H6; on passing a mixture of BF3 and H2 (ratio=1:2) over powdered NaH at about 180°C;;
In diethyl ether react. of NaH with a soln. of BF3 in ether in an autoclave (about 10 at), 24h, about 120°C;;
In mineral oil at 250-265°C;; washing with petroleum ether, extractn. of NaBH4 from the residue with liquid NH3 at -33°C;;
In neat (no solvent) byproducts: B2H6; on passing a mixture of BF3 and H2 (ratio=1:2) over powdered NaH at about 180°C;;
NaSm(BH4)4 * 4 dimethoxyethane

NaSm(BH4)4 * 4 dimethoxyethane

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

[Sm(BH4)3(tetrahydrofuran)3]

[Sm(BH4)3(tetrahydrofuran)3]

Conditions
ConditionsYield
With tetrahydrofuran In neat (no solvent) byproducts: DME; 140-160°C, vac., 2 h; extn. (THF), filtration off of NaBH4, distn. off of solvent; elem. anal.;A n/a
B 89%
Trimethyl borate
121-43-7

Trimethyl borate

sodium hydride
7646-69-7

sodium hydride

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

sodium tetramethoxyborate
18024-69-6

sodium tetramethoxyborate

Conditions
ConditionsYield
In tetrahydrofuran with excess NaH; at 65°C;A 83%
B n/a
In tetrahydrofuran on boiling in THF, pptn. of NaBH4;;
In tetrahydrofuran on boiling in THF, pptn. of NaBH4;;
sodium tetramethoxyborate
18024-69-6

sodium tetramethoxyborate

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) heating to 250-270°C, excess NaH;;78%
In neat (no solvent) heating to 250-270°C, excess NaH;;78%
In neat (no solvent) molar ratio NaH:NaB(OCH3)4=4:1, 250.C;; 91% NaBH4;;66%
In neat (no solvent) molar ratio NaH:NaB(OCH3)4=4:1, 250.C;; 91% NaBH4;;66%
sodium trimethoxyborohydride

sodium trimethoxyborohydride

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) molar ratio NaH:NaBH(OCH3)3=3:1, 250-270°C;;78%
In neat (no solvent) heating to 250-270°C, excess NaH;;78%
In neat (no solvent) molar ratio NaH:NaBH(OCH3)3=3:1, 250-270°C;;78%
Sodium borate

Sodium borate

magnesium hydride

magnesium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
With sodium carbonate In neat (no solvent) byproducts: MgO, CO2; ball milled at room temp. for 60 min; extn. by anhyd. ethylendiamine under Ar; filtered soln. evapd. in vac. at room temp.; detn. by XRD;78%
With sodium peroxide In neat (no solvent) byproducts: MgO, H2; ball milled at room temp. for 60 min; extn. by anhyd. ethylendiamine under Ar, soln. evapd. in vac. at room temp.; detn. by XRD;67%
With sodium hydroxide In neat (no solvent) byproducts: MgO, H2; ball milled at room temp. for 60 min; extn. by anhyd. ethylendiamine under Ar; filtered soln. evapd. in vac. at room temp.; detn. by XRD;64%
In neat (no solvent) byproducts: MgO, B2O3; ball milled at room temp. for 60 min; extn. by anhyd. ethylendiamine under Ar; filtered soln. evapd. in vac. at room temp.; detn. by XRD;43%
NaNd(BH4)4 * 4 dimethoxyethane

NaNd(BH4)4 * 4 dimethoxyethane

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

neodymium borohydride * 3 tetrahydrofuran

neodymium borohydride * 3 tetrahydrofuran

Conditions
ConditionsYield
With tetrahydrofuran In neat (no solvent) byproducts: DME; 140-160°C, vac., 2 h; extn. (THF), filtration off of NaBH4, distn. off of solvent, drying (vac., 1 h); elem. anal.;A n/a
B 78%
sodium amidotrihydridoborate
148977-74-6

sodium amidotrihydridoborate

dimethylsulfide borane complex
13292-87-0

dimethylsulfide borane complex

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In tetrahydrofuran for 5h; Inert atmosphere;78%
magnesium hydride

magnesium hydride

BO2(1-)*(x)H2O*Na(1+)

BO2(1-)*(x)H2O*Na(1+)

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
for 6h; Milling;76%
sodium borate

sodium borate

hydrogen
1333-74-0

hydrogen

sodium
7440-23-5

sodium

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) react. of Na-borate with Na and H2 at 400-500°C, H2-pressure: several atm, addn. of SiO2 to separate excess Na in form of Na2SiO3;; purity up to 96%;;75%
sodium triborate

sodium triborate

hydrogen
1333-74-0

hydrogen

sodium
7440-23-5

sodium

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) react. of Na-borate with Na and H2 at 400-500°C, H2-pressure: several atm, addn. of SiO2 to separate excess Na in form of Na2SiO3;; purity up to 96%;;75%
disodium octaborate

disodium octaborate

hydrogen
1333-74-0

hydrogen

sodium
7440-23-5

sodium

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) react. of Na-borate with Na and H2 at 400-500°C, H2-pressure: several atm, addn. of SiO2 to separate excess Na in form of Na2SiO3;; purity up to 96%;;75%
sodium tetrafluoroborate
13755-29-8

sodium tetrafluoroborate

hydrogen
1333-74-0

hydrogen

sodium
7440-23-5

sodium

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In further solvent(s) introduction of dry H2 under pressure in a dispersion of Na in an inert solvent at 275°C, simultanuous addn. of NaBF4;;75%
In further solvent(s) introduction of dry H2 under pressure in a dispersion of Na in an inert solvent at 250-350°C, simultanuous addn. of NaBF4;;
Sodium borate

Sodium borate

hydrogen
1333-74-0

hydrogen

sodium
7440-23-5

sodium

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) react. of Na-borate with Na and H2 at 400-500°C, H2-pressure: several atm, addn. of SiO2 to separate excess Na in form of Na2SiO3;; purity up to 96%;;75%
borane-THF
14044-65-6

borane-THF

sodium amidotrihydridoborate
148977-74-6

sodium amidotrihydridoborate

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In tetrahydrofuran at 20℃; for 5h; Inert atmosphere;75%
sodium tetrahydroxyborate

sodium tetrahydroxyborate

Mg17Al12

Mg17Al12

A

aluminum oxide
1333-84-2, 1344-28-1

aluminum oxide

B

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
for 20h; Milling; Inert atmosphere;A n/a
B 72%
sodium yttrium hydroborate*4 1,2-dimethoxyethane

sodium yttrium hydroborate*4 1,2-dimethoxyethane

3-ethylpentan-3-ol
597-49-9

3-ethylpentan-3-ol

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

ytrrium tetrahydridoborate
72033-96-6

ytrrium tetrahydridoborate

C

bis(3-ethyl-3-pentoxy)borane
144782-40-1

bis(3-ethyl-3-pentoxy)borane

Conditions
ConditionsYield
In tetrahydrofuran byproducts: H2; under inert atm.; excess of alcohol in THF added dropwise at room temp. to stirred soln. of tetrahydroborate complex in THF (accompanied by vigorous gas evolution); stirring was continued for 1 h; mixt. allowed to stand for the reaction to be completed; within 5 ds ppt. sepd. by filtration (identified as NaBH4 by X-ray diffraction and IR spectroscopy); filtrate was distd. (vac., 0.1 mmHg) at room temp. to remove solvent and at 50°C; residue pumped out at 100-115°C; volatile collected ...;A 70%
B n/a
C 69%
tetraphenylphosphonium tetrahydroborate
37080-36-7

tetraphenylphosphonium tetrahydroborate

NaLu(BH4)4*(1,2-dimethoxyethane)4

NaLu(BH4)4*(1,2-dimethoxyethane)4

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

(Ph4P)[Lu(BH4)4]

(Ph4P)[Lu(BH4)4]

Conditions
ConditionsYield
In dichloromethane CH2Cl2 was added to mixt. NaLu(BH4)4*4DME andPh4PBH4 and stirred for several minutes; NaBH4 was filtered off, soln. was concd., Et2O was added, ppt. was separated, washed with Et2O and dried in vac.; elem. anal.;A n/a
B 68.5%
NaZr(BH4)5*3(1,2-dimethoxyethane)

NaZr(BH4)5*3(1,2-dimethoxyethane)

3-ethylpentan-3-ol
597-49-9

3-ethylpentan-3-ol

A

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

B

zirconium(IV) borohydride

zirconium(IV) borohydride

C

bis(3-ethyl-3-pentoxy)borane
144782-40-1

bis(3-ethyl-3-pentoxy)borane

Conditions
ConditionsYield
In tetrahydrofuran byproducts: H2; under inert atm.; excess of alcohol in THF added dropwise at room temp. to stirred soln. of tetrahydroborate complex in THF (accompanied by vigorous gas evolution); stirring was continued for 1 h; mixt. allowed to stand for the reaction to be completed; within 5 ds ppt. sepd. by filtration (identified as NaBH4 by X-ray diffraction and IR spectroscopy); filtrate was distd. (vac., 0.1 mmHg) at room temp. to remove solvent and at 50°C; residue pumped out at 100-115°C; volatile collected ...;A 66%
B n/a
C 65%
BO2(1-)*(x)H2O*Na(1+)

BO2(1-)*(x)H2O*Na(1+)

hydrogen
1333-74-0

hydrogen

sodium hydroxide
1310-73-2

sodium hydroxide

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
With aluminium at 579.84℃; under 17251.7 Torr;65%
boron trioxide

boron trioxide

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) heating to >330°C for 20-48h;;60%
In neat (no solvent) heating to >330°C for 20-48h;;60%
With catalyst: Na-alcoholate In neat (no solvent) at about 350°C;;
boron trioxide

boron trioxide

sodium hydride
7646-69-7

sodium hydride

A

sodium metaborate

sodium metaborate

B

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
In neat (no solvent) on trituration at 330-350°C for 20-48h;;A n/a
B 60%
In neat (no solvent) on trituration at 330-350°C for 20-48h;;A n/a
B 60%
heating at 330 - 350°C;
heating at 330 - 350°C;
sodium metaborate

sodium metaborate

sodium hydride
7646-69-7

sodium hydride

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Conditions
ConditionsYield
With silica gel In solid powders ball milled for 4 h at 400 rpm, SiO2 added, ball-milled for 2 h more, pressed into pellet under 10, 20 or 30 MPa in Ar-filled box, calcined under 0.1 MPa Ar at 480°C for 5 h; extd. by isopropyl amine in modified Soxlet apparatus for 3 h; filtered,evapd. at 50°C;32%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

calcium chloride

calcium chloride

calcium borohydride

calcium borohydride

Conditions
ConditionsYield
In tetrahydrofuran byproducts: sodium chloride; under N2, soln. of CaCl2 and NaBH4 (molar ratio 1:1) in THF stirred with glass beads at 67°C (refluxed) for 1 h;100%
In tetrahydrofuran byproducts: sodium chloride; under N2, soln. of CaCl2 and NaBH4 (molar ratio 1:1) in THF stirred with glass beads at 25°C for 8 h;99%
In tetrahydrofuran byproducts: sodium chloride; under N2, soln. of CaCl2 and NaBH4 (molar ratio 1:1) in THF stirred with magnetic stirrer at 67°C (refluxed) for 8i h;96%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

iodine
7553-56-2

iodine

diborane
14452-61-0

diborane

Conditions
ConditionsYield
byproducts: H2, NaI; Interaction of initial cryst. materials in molar ratio NaBH4:I2 = 1.35 under mechanical activation with a vibration ball mill (dry N2, atm. pressure, 25°C).; Detn. of gas phase formed by infrared and mass spectroscopy, and gas volumetric anal.;100%
byproducts: H2, NaI; Interaction of initial cryst. materials in molar ratio NaBH4:I2 = 1.5 under mechanical activation with a vibration ball mill (dry N2, atm. pressure, 25°C).; Detn. of gas phase formed by infrared and mass spectroscopy, and gas volumetric anal.;97.7%
Kinetics; byproducts: H2, NaI; Interaction of initial cryst. materials in molar ratio NaBH4:I2 = 2.5 under mechanical activation with a vibration ball mill (dry N2, atm. pressure, 25°C).; Detn. of gas phase formed by infrared and mass spectroscopy, and gas volumetric anal.;94%
Kinetics; byproducts: H2, NaI; Interaction of initial cryst. materials in molar ratio NaBH4:I2 = 2.0 under mechanical activation with a vibration ball mill (dry N2, atm. pressure, 25°C).; Detn. of gas phase formed by infrared and mass spectroscopy, and gas volumetric anal.;88.7%
byproducts: H2, HI; Grinding of initial materials (molar ratio = 1) while being cooled withliq. N2, thorough mixing, transferring of mixt. to a thermographic ampoule and heating in vac. or N2.; Sepn. of gas mixt. by fractional condensation. Detn. of composition after the thermography by gas volumetric anal.;
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

lithium bromide
7550-35-8

lithium bromide

lithium borohydride

lithium borohydride

Conditions
ConditionsYield
In tetrahydrofuran byproducts: sodium bromide; under N2, soln. of LiBr and NaBH4 (molar ratio 1:1) in THF stirred withglass beads at 67°C (refluxed) for 8 h;100%
In tetrahydrofuran byproducts: sodium bromide; under N2, soln. of LiBr and NaBH4 (molar ratio 1:1) in THF stirred withmagnetic stirrer at 67°C (refluxed) for 16 h;99%
In diethyl ether byproducts: sodium bromide; under N2, soln. of LiBr in Et2O stirred with magnetic stirrer for 2 min, 1 equiv of NaBH4 introduced, maintained at 35°C with stirring for 32 h;99%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

lithium chloride

lithium chloride

lithium borohydride

lithium borohydride

Conditions
ConditionsYield
In tetrahydrofuran byproducts: sodium chloride; under N2, soln. of LiCl and NaBH4 (molar ratio 1:1) in THF stirred withglass beads at 25°C for 24 h or at 67°C (refluxed) for 10h;100%
extraction with ether; purity: 97-98 %;75%
In tetrahydrofuran byproducts: sodium chloride; under N2, soln. of LiCl and NaBH4 (molar ratio 1:1) in THF stirred withmagnetic stirrer at 67°C (refluxed) for 48 h;65%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

benzo-2-chloro-1,3,2-diazaborolane
91159-98-7

benzo-2-chloro-1,3,2-diazaborolane

2,3-dihydro-1H-1,3,2-benzodiazaborole
89799-28-0

2,3-dihydro-1H-1,3,2-benzodiazaborole

Conditions
ConditionsYield
In benzene recrystn. from benzene;100%
sulfur
10544-50-0

sulfur

sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

ammonia
7664-41-7

ammonia

ammonia borane complex
10043-11-5

ammonia borane complex

Conditions
ConditionsYield
In ammonia to NaBH4 in a flask at -40°C NH3 is condensed, then slowly S8 isadded (5 h), to the mixt. (after 3 h) CH2Cl2 is added, then the mixt. is warmed to room temp.; residue is extd. with CH2Cl2, the soln. is evapd., elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

[(μ-η(2)-η(3)-HC*C-CH2)CoMo(Cp)(CO)5](BF4)

[(μ-η(2)-η(3)-HC*C-CH2)CoMo(Cp)(CO)5](BF4)

(μ-η(2)-η(2)-HC*CCH3)CoMo(Cp)(CO)5
126979-16-6

(μ-η(2)-η(2)-HC*CCH3)CoMo(Cp)(CO)5

Conditions
ConditionsYield
In dichloromethane Ar-atmosphere; addn. of excess of NaBH4 to soln. of complex at 0°C; extn. (ether), washing org. layer by H2O, drying (MgSO4), evapn.; elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

IrH2(CH3CN)(C6H5P(CH2CH2CH2P(C6H11)2)2)(1+)*BF4(1-)={IrH2(CH3CN)(C6H5P((CH2)3P(C6H11)2)2)}{BF4}
103746-20-9, 103833-40-5

IrH2(CH3CN)(C6H5P(CH2CH2CH2P(C6H11)2)2)(1+)*BF4(1-)={IrH2(CH3CN)(C6H5P((CH2)3P(C6H11)2)2)}{BF4}

IrH3(C6H5P(CH2CH2CH2P(C6H11)2)2)*C2H5OH
145036-85-7

IrH3(C6H5P(CH2CH2CH2P(C6H11)2)2)*C2H5OH

Conditions
ConditionsYield
In tetrahydrofuran nitrogen atmosphere; NaBH4 added to the Ir complex in THF; mixt. stirred for 20 min; addn. of ethanol, stirring (1 h); removal of the solvent (red. pressure); residue dissolved in THF, filtration; elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

1,3-diferrocenyl-2-propen-1-one
105404-21-5

1,3-diferrocenyl-2-propen-1-one

rac-1,3-diferrocenylprop-2-en-1-ol
72971-83-6

rac-1,3-diferrocenylprop-2-en-1-ol

Conditions
ConditionsYield
In 1,4-dioxane; methanol NaBH4 added to soln. of Fe complex (stirring); stirred (14 h); H2O added; cooled (7-8°C); ppt. filtered; washed (H2O); dried (room temp.); recrystd. (hexane); elem.anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

Pt2Me2(μ-Cl)(μ-N,N'-bis[(2-diphenylphosphino)phenyl]formamidinate)
441072-64-6

Pt2Me2(μ-Cl)(μ-N,N'-bis[(2-diphenylphosphino)phenyl]formamidinate)

Pt2(methyl)2(μ-H)(μ-N,N'-bis[2-(diphenylphosphino)phenyl]formamidinate)
441072-56-6

Pt2(methyl)2(μ-H)(μ-N,N'-bis[2-(diphenylphosphino)phenyl]formamidinate)

Conditions
ConditionsYield
In methanol; dichloromethane under N2 atm. to soln. Pt2Me2(μ-Cl)(μ-dpfam) in CH2Cl2 was addedNaBH4 and MeOH at 0°C and mixt. was stirred for 1 h; solvents were removed under reduced pressure, residue was extd. with CH2Cl2 and filtered, soln. was evapd.; elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

(η(5)-cyclopentadienyl)OsCl(triisopropylphosphine)2
196520-48-6

(η(5)-cyclopentadienyl)OsCl(triisopropylphosphine)2

OsH(η(5)-C5H5)(PiPr3)2
196520-49-7

OsH(η(5)-C5H5)(PiPr3)2

Conditions
ConditionsYield
With MeOH In toluene air-free atmosphere; stirring (room temp., 15 min); filtering, evapn., pentane addn., filtering, evapn.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

borane-THF
14044-65-6

borane-THF

diphosphane-borane
186336-54-9

diphosphane-borane

sodium 1,1,2-tris(borane)-1,2,2-trihydrogendiphosphide
186336-57-2

sodium 1,1,2-tris(borane)-1,2,2-trihydrogendiphosphide

Conditions
ConditionsYield
In tetrahydrofuran byproducts: H2, Na2[P2H2(BH3)4]; N2 atm.; molar ratio P2H4BH3:NaBH4 1:1, cooling (-78 to -196°C), stirring (4 h), heating (-78°C, 3 h), stirring (room temp., 6 h); crystn. (-78°C, several d);100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

[(5,7-dimethyl-6-anthracyl-1,4,8,11-tetraazacyclotetradeca-4,7-diene)nickel(II)] nitrate iodide

[(5,7-dimethyl-6-anthracyl-1,4,8,11-tetraazacyclotetradeca-4,7-diene)nickel(II)] nitrate iodide

sodium perchlorate

sodium perchlorate

water
7732-18-5

water

[(5,7-dimethyl-6-anthracyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)] perchlorate dihydrate

[(5,7-dimethyl-6-anthracyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)] perchlorate dihydrate

Conditions
ConditionsYield
In methanol a 15 equiv of NaBH4 was added to a soln. of complex in methanol, the mixt. was allowed to stir at room temp. for 2 h, ppt. was filtered off, dissolved in H2O, aq. satd. NaClO4 was added dropwise, cooled; ppt. was filtered, washed with ice-cold water and then ether; elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

[(5,7-dimethyl-6-(p-hydroxymethylbenzyl)-1,4,8,11-tetraazacyclotetradeca-4,7-diene)nickel(II)] nitrate iodide

[(5,7-dimethyl-6-(p-hydroxymethylbenzyl)-1,4,8,11-tetraazacyclotetradeca-4,7-diene)nickel(II)] nitrate iodide

sodium perchlorate

sodium perchlorate

[(5,7-dimethyl-6-(p-hydroxymethylbenzyl)-1,4,8,11-tetraazacyclotetradecane)nickel(II)] perchlorate

[(5,7-dimethyl-6-(p-hydroxymethylbenzyl)-1,4,8,11-tetraazacyclotetradecane)nickel(II)] perchlorate

Conditions
ConditionsYield
In methanol a 15 equiv of NaBH4 was added to a soln. of complex in methanol, the mixt. was allowed to stir at room temp. for 2 h, ppt. was filtered off, dissolved in H2O, aq. satd. NaClO4 was added dropwise, cooled; ppt. was filtered, washed with ice-cold water and then ether;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

(2,6-bis[(di-t-butylphosphino)methyl]phenyl)chloronickel
60426-33-7

(2,6-bis[(di-t-butylphosphino)methyl]phenyl)chloronickel

(2,6-bis[(di-t-butylphosphino)methyl]phenyl)hydridonickel
60399-53-3

(2,6-bis[(di-t-butylphosphino)methyl]phenyl)hydridonickel

Conditions
ConditionsYield
In ethanol; benzene excess of NaBH4, stirring in C6H6/EtOH=1:1 for 20 h at 20°C, addn. of further NaBH4. stirring for 3 h; addn. of water and C6H6, evapn. of C6H6-layer;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

[2,6-bis(2-(2-mercaptophenyl)1-methyl-2-azaethenyl)pyridine]zinc(II)
39007-30-2, 52019-98-4

[2,6-bis(2-(2-mercaptophenyl)1-methyl-2-azaethenyl)pyridine]zinc(II)

[2,6-bis(1-(2-mercaptoanilino)ethyl)pyridine]zinc(II)
354115-72-3

[2,6-bis(1-(2-mercaptoanilino)ethyl)pyridine]zinc(II)

Conditions
ConditionsYield
In ethanol; N,N-dimethyl-formamide all manipulations under Ar atm.; soln. of NaBH4 in EtOH/DMF (1/4) added dropwise to soln. of complex in DMF at 0°C, stirred at room temp for 2 h; DMF/EtOH removed in vac., residue dissolved in MeOH, pptd. by addn. of water; elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

(1S,2R,3S,4R)-3-methoxymethyl-2-triphenylstannylbicyclo[2.2.1]heptane(-)
203380-20-5

(1S,2R,3S,4R)-3-methoxymethyl-2-triphenylstannylbicyclo[2.2.1]heptane(-)

iodine
7553-56-2

iodine

diphenyl[(1S,2R,3S,4R)-3-(1-methoxymethyl)bicyclo[2.2.1]heptan-2-yl]tin hydride
203380-22-7

diphenyl[(1S,2R,3S,4R)-3-(1-methoxymethyl)bicyclo[2.2.1]heptan-2-yl]tin hydride

Conditions
ConditionsYield
In dichloromethane I2 addn. to Sn-compd. soln. (DCM), stirring 1 h at room temp., concn. (reduced pressure), B-compd. soln. (EtOH), after 1 h mixt. partitioning between satd. aq. NH4Cl and Et2O, aq. phase extn. (Et2O), extract drying (MgSO4), concn. (reduced pressure);100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

[(5,7-dimethyl-6-benzyl-1,4,8,11-tetraazacyclotetradeca-4,7-diene)nickel(II)] nitrate iodide
852290-93-8

[(5,7-dimethyl-6-benzyl-1,4,8,11-tetraazacyclotetradeca-4,7-diene)nickel(II)] nitrate iodide

sodium perchlorate

sodium perchlorate

water
7732-18-5

water

[(5,7-dimethyl-6-benzyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)] perchlorate monohydrate

[(5,7-dimethyl-6-benzyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)] perchlorate monohydrate

Conditions
ConditionsYield
In methanol a large excess of NaBH4 was added to a soln. of complex in methanol, themixt. was allowed to stir at room temp. for 2 h, ppt. was filtered off, dissolved in H2O, aq. satd. NaClO4 was added dropwise, cooled; ppt. was filtered, washed with ice-cold water and then ether; elem. anal.;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

diphenyl[(1S,2R,3S,4R)-3-hydroxymethylbicyclo[2.2.1]heptan-2-yl]tin iodide

diphenyl[(1S,2R,3S,4R)-3-hydroxymethylbicyclo[2.2.1]heptan-2-yl]tin iodide

diphenyl[(1S,2R,3S,4R)-3-hydroxymethylbicyclo[2.2.1]heptan-2-yl]tin hydride
203380-24-9

diphenyl[(1S,2R,3S,4R)-3-hydroxymethylbicyclo[2.2.1]heptan-2-yl]tin hydride

Conditions
ConditionsYield
In ethanol B-compd. soln. addn. to Sn-compd. soln. at ambient temp., mixt. concn. (reduced pressure) after 30 min, residue partitionation between satd. aq.NH4Cl and Et2O, aq. phase extn. (Et2O), org. extract drying (MgSO4), co ncn. (reduced pressure);100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

1,1,1,3',3',3'-hexafluoro-propanol
920-66-1

1,1,1,3',3',3'-hexafluoro-propanol

Sodium Tris(1,1,1,3,3,3-hexafluoroisopropoxy)borohydride

Sodium Tris(1,1,1,3,3,3-hexafluoroisopropoxy)borohydride

Conditions
ConditionsYield
In tetrahydrofuran at 0℃;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

carbonylchlorohydrido(4,5-bis((diisopropylphosphino)methyl)acridine)ruthenium(II)
1101230-25-4

carbonylchlorohydrido(4,5-bis((diisopropylphosphino)methyl)acridine)ruthenium(II)

C28H43BClNOP2Ru

C28H43BClNOP2Ru

Conditions
ConditionsYield
In tetrahydrofuran at 20℃; for 2h; Inert atmosphere;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

1,2-dimethoxyethane
110-71-4

1,2-dimethoxyethane

5-nitro-2H-tetrazole
55011-46-6

5-nitro-2H-tetrazole

A

[Na(1,,2-dimethoxyethane)3][bis(5-nitro-2H-tetrazolyl)dihydroborate]

[Na(1,,2-dimethoxyethane)3][bis(5-nitro-2H-tetrazolyl)dihydroborate]

B

hydrogen
1333-74-0

hydrogen

Conditions
ConditionsYield
at 20℃; for 4h; Inert atmosphere;A 100%
B 3.9 mmol
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

1,2-dimethoxyethane
110-71-4

1,2-dimethoxyethane

5-(trinitromethyl)-2H-tetrazole
75393-84-9

5-(trinitromethyl)-2H-tetrazole

A

[Na(1,,2-dimethoxyethane)3][bis(5-(trinitromethyl)-2H-tetrazolyl)dihydroborate]

[Na(1,,2-dimethoxyethane)3][bis(5-(trinitromethyl)-2H-tetrazolyl)dihydroborate]

B

hydrogen
1333-74-0

hydrogen

Conditions
ConditionsYield
at 20℃; for 4h; Inert atmosphere;A 100%
B 3.8 mmol
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

1,2-dimethoxyethane
110-71-4

1,2-dimethoxyethane

5-(fluorodinitromethyl)tetrazole
75393-85-0

5-(fluorodinitromethyl)tetrazole

A

[Na(1,,2-dimethoxyethane)3][bis(5-(fluorodinitromethyl)-2H-tetrazolyl)dihydroborate]

[Na(1,,2-dimethoxyethane)3][bis(5-(fluorodinitromethyl)-2H-tetrazolyl)dihydroborate]

B

hydrogen
1333-74-0

hydrogen

Conditions
ConditionsYield
at 20℃; for 4h; Inert atmosphere;A 100%
B 3.7 mmol
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

1,2-dimethoxyethane
110-71-4

1,2-dimethoxyethane

3,5-dinitro-1H-1,2,4-triazole
26621-32-9

3,5-dinitro-1H-1,2,4-triazole

A

[Na(1,,2-dimethoxyethane)3][bis(3,5-dinitro-1H-1,2,4-triazolyl)dihydroborate]

[Na(1,,2-dimethoxyethane)3][bis(3,5-dinitro-1H-1,2,4-triazolyl)dihydroborate]

B

hydrogen
1333-74-0

hydrogen

Conditions
ConditionsYield
at 20℃; for 4h; Inert atmosphere;A 100%
B 4.1 mmol
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

trinitromethane
517-25-9

trinitromethane

sodium (trinitromethyl)borate

sodium (trinitromethyl)borate

Conditions
ConditionsYield
In 1,2-dimethoxyethane Schlenk technique; Inert atmosphere;100%
In tetrahydrofuran at 20℃; for 0.75h;
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

trimethylsilyl cyanide
7677-24-9

trimethylsilyl cyanide

sodium dicyanodihydridoborate
88503-36-0

sodium dicyanodihydridoborate

Conditions
ConditionsYield
for 48h; Inert atmosphere; Reflux;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

cis-α-dichloro {N,N′-[1,2-phenylenebis(methylene)]bis[2-(diphenylphosphino)ethylamine]}ruthenium(II)

cis-α-dichloro {N,N′-[1,2-phenylenebis(methylene)]bis[2-(diphenylphosphino)ethylamine]}ruthenium(II)

hydrideborohydride {N,N′-[1,2-phenylenebis(methylene)]bis[2-(diphenylphosphino)ethylamine]}ruthenium(II)

hydrideborohydride {N,N′-[1,2-phenylenebis(methylene)]bis[2-(diphenylphosphino)ethylamine]}ruthenium(II)

Conditions
ConditionsYield
With ethanol for 1h; Inert atmosphere; Reflux;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

[bis(2-diphenylphosphinophenyl)amide]PdCl

[bis(2-diphenylphosphinophenyl)amide]PdCl

C36H29NP2Pd

C36H29NP2Pd

Conditions
ConditionsYield
In tetrahydrofuran; benzene-d6 at 20℃; for 1h; Inert atmosphere;100%
sodium tetrahydroborate
16940-66-2

sodium tetrahydroborate

(S)-(+)-β-phenyl-β-alanine methyl ester hydrochloride

(S)-(+)-β-phenyl-β-alanine methyl ester hydrochloride

C9H12BNO2

C9H12BNO2

Conditions
ConditionsYield
With zinc(II) chloride In tetrahydrofuran for 4h; Reagent/catalyst; Reflux;99.6%

16940-66-2Relevant articles and documents

A facile solvent-free method for NaBH4 and Na2B12H12 synthesis

He, Liqing,Fu, Yanda,Wu, Dong,Zhang, Dehui,Cheng, Hua,Lin, Huaijun,Li, Xiangnan,Xiong, Wei,Zhu, Qing,Deng, Yonghong,Shao, Huaiyu,Li, Hai-Wen,Zhao, Xingzhong,Lu, Zhouguang

, p. 16 - 21 (2018)

Sodium tetrahydroborate (NaBH4) and dodecahydro-closo-dodecaborate (Na2B12H12) are both important inorganic compounds presenting multiple applications. Nevertheless, multistep and complicated conditions are usually demanded for their synthesis. In order to simplify the synthesis processes, we design a novel and facile solvent-free method for synthesizing NaBH4 or Na2B12H12 from NaNH2 and B10H14. The product of either NaBH4 or Na2B12H12 is manipulable by simply adjusting the ratio of NaNH2 to B10H14. The reaction equations of synthesizing NaBH4 and Na2B12H12 are proposed and verified, and the reaction pathways are elucidated. The findings here supply new insight to synthesize metal dodecaborates using the strategy of equal electron body for the first time and may shed light on synthesis of small metal B-H compounds from large B-H clusters.

Synthesis of NaBH4 based on a solid-state reaction under Ar atmosphere

Zhang, Hanping,Zheng, Shiyou,Fang, Fang,Chen, Guorong,Sang, Ge,Sun, Dalin

, p. 352 - 355 (2009)

Sodium borohydride, NaBH4, was successfully synthesized via solid-state reaction under Ar instead of H2 atmosphere. A 4NaH-NaBO2-2SiO2 ternary mixture was first ball-milled and pressed into pellet, and then calc

Supersilylated tetraphosphene derivatives M2[t-Bu 3SiPPPPSi-t-Bu3] (M = Li, Na, Rb, Cs) and Ba[t-Bu 3SiPPPPSi-t-Bu3]: Reactivity and Cis-trans isomerization

Lorbach, Andreas,Nadj, Andor,Tuellmann, Sandor,Dornhaus, Franz,Schoedel, Frauke,Saenger, Inge,Margraf, Guenter,Bats, Jan W.,Bolte, Michael,Holthausen, Max C.,Wagner, Matthias,Lerner, Hans-Wolfram

, p. 1005 - 1017 (2009)

The tetraphosphenediides M2[t-Bu3SiPPPPSi-t-Bu 3] (M = Li, Na, K) were accessible by the reaction of P4 with the silanides M[Si-t-Bu3] (M = Li, Na, K), whereas M 2[t-Bu3SiPPPPSi-

A simple and efficient way to synthesize unsolvated sodium octahydrotriborate

Huang, Zhenguo,King, Graham,Chen, Xuenian,Hoy, Jason,Yisgedu, Teshome,Lingam, Hima K.,Shore, Sheldon G.,Woodward, Patrick M.,Zhao, Ji-Cheng

, p. 8185 - 8187 (2010)

A simple and efficient way to synthesize unsolvated sodium octahydrotriborate has been developed. This method avoids the use of dangerous starting materials and significantly simplifies the reaction setup, thus enabling convenient large-scale synthesis. The structure of the unsolvated compound has been determined through powder X-ray diffraction.

Structure and properties of NaBH4·2H2O and NaBH4

Filinchuk, Yaroslav,Hagemann, Hans

, p. 3127 - 3133 (2008)

NaBH4·2H2O and NaBH4 were studied by single-crystal Xray diffraction and vibrational spectroscopy. In NaBH 4·2H2O, the BH4- anion has a nearly ideal tetrahedral geometry and is bridged with two Na+ ions through the tetrahedral edges. The structure does not contain classical hydrogen bonds, but reveals strong dihydrogen bonds of 1.77-1.95 A. Crystal structures and vibrational spectra of NaBr·2H2O and NaBH 4·2H2O reveal many similarities. The unit cell volume of NaBH4·2H2O increases linearly with temperature between 200 and 313 K. At 313-315 K, the hydrate decomposes into NaBH4 and H2O, which react to release hydrogen. Wiley-VCH Verlag GmbH & Co. KGaA, 2008.

-

Keller,P.C.

, p. 1231 (1969)

-

ANIONIC ZIRCONIUM AND HAFNIUM BOROHYDRIDE COMPLEXES

Makhaev, V. D.,Borisov, A. P.,Boiko, G. N.,Tarasov, B. P.

, (1990)

Zirconium and hafnium tetrachlorides react with NaBH4 in dimethoxyethane (DME) to give .These compounds react with Bu4NBH4 and Ph4PBH4 to give (R4E).Bidentate and tridentate BH4(1-) occur in (1-) according to IR spectr

Preparation of sodium borohydride by the reaction of MgH2 with dehydrated borax through ball milling at room temperature

Li,Morigazaki,Liu,Suda

, p. 232 - 236 (2003)

A convenient method was developed to synthesize NaBH4 by the reaction of MgH2 with Na2B4O7 through ball milling at room temperature. In order to improve the sodium borohydride yield, Na compounds were added to compensate the Na insufficiency in reactants when MgH2 instead of NaH was used as the reducing agent. It was found that Na2CO3 addition was better than NaOH or Na2O2 addition in increasing the borohydride yield.

Tris(dithiolene) complexes of neodymium and cerium: Mononuclear species, chains, and honeycomb networks

Roger, Mathieu,Arliguie, Therese,Thuery, Pierre,Fourmigue, Marc,Ephritikhine, Michel

, p. 584 - 593 (2005)

Reactions of Ln(BH4)3(THF)3 (Ln = Nd, Ce) and M2dddt (M = Na, K; dddt = 5,6-dihydro-1,4-dithiine-2,3- dithiolate) in THF or pyridine gave, after addition of 18c6 (18-crown-6), several crystalline compounds which all contain the tris(dithiolene) Ln(dddt)3 unit. Crystals of [Na(18c6)(py)2] 2[Na(18c6)(py)][Nd(dddt)3(py)]·3py (1·3py) are built up from discrete mononuclear cationic and anionic species whereas crystals of {[Na(18c6)(py)2]0.5[Na(18c6)(py) 1.5][Na1.5Nd(dddt)3]}∞ (2) are composed of discrete [Na(18c6)(py)x]+ cations and polymeric anionic two-dimensional layers in which the Nd(dddt)3 units are linked to three neighbors by sodium atoms to form a honeycomb network. Analysis of the temperature dependence of the molar magnetic susceptibility of 2 shows that χMT decreases from 1.63 cm3 K mol -1 at 300 K down to 0.6 cm3 K mol-1 at 5 K, due to the crystal-field splitting of the 4I9/2 free-ion state. Complexes {[Na3(18c6)1.5Nd(dddt) 3(THF)]·3THF}∞ (3·3THF) and {[K 3(18c6)1.5Nd(dddt)3(py)]·3py} ∞ (4·3py) exhibit neutral polymeric layers with the Nd(dddt)3 units linked by M2(18c6) fragments. In the cerium compound {[Na2(18c6)Na(py)2Ce(dddt) 3(py)]·3py}∞ (5·3py), each Ce(dddt)3 unit is linked to two neighbors only by Na 2(18c6) moieties, giving infinite zigzag chains.

Hough, W. V.,Edwards, L. J.,McElroy, A. D.

, p. 1828 - 1829 (1958)

Sodium borohydride formation when Mg reacts with hydrous sodium borates under hydrogen

Liu, Bin Hong,Li, Zhou Peng,Zhu, Jing Ke

, p. L16-L20 (2009)

In this work, we explored the possibility of NaBH4 synthesis when Mg reacted with hydrous sodium borates under hydrogen. It was found that Mg could react with the water in molten hydrous borates to form MgO and release hydrogen, which can be us

Challenges in the synthetic routes to Mn(BH4)2: Insight into intermediate compounds

Tumanov, Nikolay A.,Safin, Damir A.,Richter, Bo,?odziana, Zbigniew,Jensen, Torben R.,Garcia, Yann,Filinchuk, Yaroslav

, p. 6571 - 6580 (2015)

We have studied the reaction of MnCl2 with MBH4 (M = Li+, Na+, K+) in Et2O. Crystal structures of two new intermediates, named [{M(Et2O)2}Mn2(BH4)5] (M = Li+, Na+), were elucidated by X-ray diffraction. Mn(BH4)2 in a mixture with LiBH4 or NaBH4 forms upon the solvent removal in a vacuum. [{M(Et2O)2}Mn2(BH4)5] contains 2D layers formed by Mn and BH4 groups, linked through the alkali metal atoms coordinated to Et2O. The loss of the solvent molecules leads to the segregation of the partially amorphous or nanocrystalline LiBH4/NaBH4 and a creation of the 3D framework of the crystalline Mn(BH4)2. While using LiBH4 led to Mn(BH4)2 contaminated with LiCl, presumably due to an efficient trapping of the latter salt by the [Mn(BH4)2-Et2O] system, the reaction with NaBH4 produced chlorine-free Mn(BH4)2 accompanied with NaBH4. Using KBH4 led to the formation of K2Mn(BH4)4 as a second phase. Two pyridine-containing solvomorphs, [Mn(py)3(BH4)2] and [Mn(py)4(BH4)2]·2py, were isolated in pure form. However, Mn(BH4)2 partly decomposes upon removal of pyridine molecules. This journal is

Hydroboration Reaction and Mechanism of Carboxylic Acids using NaNH2(BH3)2, a Hydroboration Reagent with Reducing Capability between NaBH4and LiAlH4

Wang, Jin,Ju, Ming-Yue,Wang, Xinghua,Ma, Yan-Na,Wei, Donghui,Chen, Xuenian

supporting information, p. 5305 - 5316 (2021/04/12)

Hydroboration reactions of carboxylic acids using sodium aminodiboranate (NaNH2[BH3]2, NaADBH) to form primary alcohols were systematically investigated, and the reduction mechanism was elucidated experimentally and computationally. The transfer of hydride ions from B atoms to C atoms, the key step in the mechanism, was theoretically illustrated and supported by experimental results. The intermediates of NH2B2H5, PhCH= CHCOOBH2NH2BH3-, PhCH= CHCH2OBO, and the byproducts of BH4-, NH2BH2, and NH2BH3- were identified and characterized by 11B and 1H NMR. The reducing capacity of NaADBH was found between that of NaBH4 and LiAlH4. We have thus found that NaADBH is a promising reducing agent for hydroboration because of its stability and easy handling. These reactions exhibit excellent yields and good selectivity, therefore providing alternative synthetic approaches for the conversion of carboxylic acids to primary alcohols with a wide range of functional group tolerance.

Realizing facile regeneration of spent NaBH4 with Mg-Al alloy

Zhong, Hao,Ouyang, Liuzhang,Zeng, Meiqin,Liu, Jiangwen,Wang, Hui,Shao, Huaiyu,Felderhoff, Michael,Zhu, Min

supporting information, p. 10723 - 10728 (2019/05/06)

The regeneration of sodium borohydride (NaBH4) is crucial to form a closed cycle after it either supplies hydrogen energy via a hydrolysis process or provides energy through electron transfer at the anode of direct borohydride fuel cells (DBFCs). In both of these cases, the spent fuels are NaB(OH)4 from NaBO2 aqueous solution. However, the current regeneration process from (NaB(OH)4)·xH2O to form NaBH4 by reduction reaction and calcination at high temperature with metal hydrides as reducing agents is very expensive. In this work, we developed a simple regeneration process via ball milling with Mg-Al alloys as the reducing agent for NaB(OH)4 under an argon atmosphere. Under optimized conditions, a high yield of about 72% of NaBH4 could be obtained. Mechanistic study showed that all the hydrogen atoms from NaB(OH)4 remain in NaBH4 and no additional hydrogen sources are needed for the reduction process. The inexpensive Mg-Al alloy works as a reducing agent transforming the H+ to H- in NaBH4. This approach demonstrates a ~20-fold cost reduction compared with the method using metal hydrides. This opens the door to the commercial implementation of simple ball milling processes for the regeneration of spent NaBH4 from NaB(OH)4 with cheap reducing agents.