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1314-85-8

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1314-85-8 Usage

Chemical Properties

Yellowish-green crystals; melts at 172°C (341°F); boils at 407–408°C (764–766°F);density 2.03 at 20°C (68 °F); soluble in carbon disulfide, benzene, and toluene, reacts with water..

Uses

Different sources of media describe the Uses of 1314-85-8 differently. You can refer to the following data:
1. Phosphorus sesquisulfide is used in in match tips.
2. Phosphorus sesquisulfide is used in making safety matches.
3. In match tips.

General Description

A yellow crystalline solid. Easily ignited by friction. Forms sulfur dioxide and phosphorus pentaoxide during combustion. Reacts with water to form phosphoric acid, a corrosive material. Used to make matches and in the manufacture of other chemicals.

Air & Water Reactions

Highly flammable.Slowly decomposed by water to form phosphoric acid and toxic hydrogen sulfide gas (H2S). May ignite on contact with water or moist air.

Reactivity Profile

PHOSPHORUS SESQUISULFIDE is a reducing agent.

Health Hazard

Different sources of media describe the Health Hazard of 1314-85-8 differently. You can refer to the following data:
1. Highly toxic: contact with water produces toxic gas, may be fatal if inhaled. Inhalation or contact with vapors, substance or decomposition products may cause severe injury or death. May produce corrosive solutions on contact with water. Fire will produce irritating, corrosive and/or toxic gases. Runoff from fire control may cause pollution.
2. Phosphorus sesquisulfide exhibited low to moderate acute oral toxicity in animals. An oral dose lethal to rabbits was reported to be 100 mg/kg (NIOSH 1986). Because of its low vapor pressure, any health hazard due to inhalation of this compound in the work place should be very low. There is no report on its acute inhalation toxicity. Its vapors may produce irritation of respiratory passage. Skin contact may cause mild irritation. It produces toxic sulfur dioxide on burning.

Fire Hazard

Produce flammable and toxic gases on contact with water. May ignite on contact with water or moist air. Some react vigorously or explosively on contact with water. May be ignited by heat, sparks or flames. May re-ignite after fire is extinguished. Some are transported in highly flammable liquids. Containers may explode when heated. Runoff may create fire or explosion hazard.

Flammability and Explosibility

Flammable

Safety Profile

Poison by ingestion. Flammable by spontaneous ignition. When heated to decomposition it emits very toxic fumes of POx and SOx. See also SULFIDES and PHOSPHORUS.

Purification Methods

Extract P4S3with CS2, filter it and evaporate it to dryness. Alternatively place it in H2O, and pass steam through it for an hour. The H2O is then removed, the solid is dried, and recrystallised from CS2 [Rogers & Gross J Am Chem Soc 74 5294 1952].

Waste Disposal

An alkaline solution is treated with laundry bleach, allowed to stand overnight, neutralized, and washed down the drain with plenty of water.

Check Digit Verification of cas no

The CAS Registry Mumber 1314-85-8 includes 7 digits separated into 3 groups by hyphens. The first part of the number,starting from the left, has 4 digits, 1,3,1 and 4 respectively; the second part has 2 digits, 8 and 5 respectively.
Calculate Digit Verification of CAS Registry Number 1314-85:
(6*1)+(5*3)+(4*1)+(3*4)+(2*8)+(1*5)=58
58 % 10 = 8
So 1314-85-8 is a valid CAS Registry Number.
InChI:InChI=1/P4S3/c5-1-2-3(1)7-4(5)6-2

1314-85-8SDS

SAFETY DATA SHEETS

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

Version: 1.0

Creation Date: Aug 13, 2017

Revision Date: Aug 13, 2017

1.Identification

1.1 GHS Product identifier

Product name Tetraphosphorus trisulfide

1.2 Other means of identification

Product number -
Other names Phosphorous sesquisulfide

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:1314-85-8 SDS

1314-85-8Synthetic route

phosphorous

phosphorous

sulfur
7704-34-9

sulfur

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

phosphorus sulfide
131105-01-6

phosphorus sulfide

C

P4S5

P4S5

tetraphosphorus tetrasulphide
39350-99-7

tetraphosphorus tetrasulphide

E

phosphorus sulfide
12037-82-0

phosphorus sulfide

Conditions
ConditionsYield
In melt vac., 10-100 mol% S, heating (1 week, 673 K); extraction (CS2), filtn.; followed by (31)P NMR;
phosphorous

phosphorous

sulfur
7704-34-9

sulfur

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

phosphorous trisulfide
131105-01-6

phosphorous trisulfide

C

phosphorus sulfide

phosphorus sulfide

D

P4S5

P4S5

E

phosphorus sulfide
12037-82-0

phosphorus sulfide

Conditions
ConditionsYield
In melt vac.,; 54 mol% S, heating (573-873 K), standing (5 weeks, room temp.); extraction (CS2), filtn.; followed by (31)P NMR;
In melt vac.,; 54 mol% S, heating (573-873 K); extraction (CS2), filtn.; followed by (31)P NMR;
phosphorous

phosphorous

sulfur
7704-34-9

sulfur

A

tetraphosphorus decasulfide
15857-57-5

tetraphosphorus decasulfide

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

C

phosphorus sulfide
12037-82-0

phosphorus sulfide

thionyl chloride
7719-09-7

thionyl chloride

phosphan
7803-51-2

phosphan

A

hydrogenchloride
7647-01-0

hydrogenchloride

B

trichlorothiophosphine
3982-91-0

trichlorothiophosphine

C

phosphorus

phosphorus

D

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In neat (no solvent) room temp.;; further unidentified liquid products;;
thionyl chloride
7719-09-7

thionyl chloride

phosphan
7803-51-2

phosphan

A

hydrogenchloride
7647-01-0

hydrogenchloride

B

phosphorus

phosphorus

C

phosphorus sulfide
1314-85-8

phosphorus sulfide

hydrogen sulfide
7783-06-4

hydrogen sulfide

phosphorus trichloride
7719-12-2, 52843-90-0

phosphorus trichloride

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
With 2-methylpyridine In not given byproducts: CH3C5H4NH(PS2Cl2), CH3C5H4NH(Cl);
sulfuryl dichloride
7791-25-5

sulfuryl dichloride

phosphan
7803-51-2

phosphan

A

hydrogenchloride
7647-01-0

hydrogenchloride

B

phosphorus

phosphorus

C

phosphorus sulfide
1314-85-8

phosphorus sulfide

phosphan
7803-51-2

phosphan

A

phosphorus

phosphorus

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

C

hydrogen sulfide
7783-06-4

hydrogen sulfide

Conditions
ConditionsYield
With sulfur with pured and dried PH3 in vacuum; at 450°C; equilibrium reaction 3-4.5 mol S for two mol PH3;
With S with pured and dried PH3 in vacuum; at 450°C; equilibrium reaction 3-4.5 mol S for two mol PH3;
phosphan
7803-51-2

phosphan

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

phosphorous

phosphorous

Conditions
ConditionsYield
With sulfuryl dichloride In neat (no solvent) react. of SO2Cl2 with dry PH3; formation of HCl, P4S3, red P, POCl3 and P2O3;;
With thionyl chloride In neat (no solvent) react. of SOCl2 with dry PH3; formation of HCl, P4S3 and red P;;
pyrosulfuryl chloride
7791-27-7

pyrosulfuryl chloride

A

hydrogenchloride
7647-01-0

hydrogenchloride

B

chlorosulfonic acid
7790-94-5

chlorosulfonic acid

C

metaphosphoric acid

metaphosphoric acid

D

phosphorus sulfide
1314-85-8

phosphorus sulfide

E

sulfur dioxide
7446-09-5

sulfur dioxide

Conditions
ConditionsYield
With hydrogen phosphide In neat (no solvent) 10°C;;
pyrosulfuryl chloride
7791-27-7

pyrosulfuryl chloride

phosphan
7803-51-2

phosphan

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In not given byproducts: HCl, SO2;
iron sulfide

iron sulfide

Sodium trimetaphosphate

Sodium trimetaphosphate

A

tetraphosphorus decasulfide
15857-57-5

tetraphosphorus decasulfide

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

C

phosphorus sulfide
12037-82-0

phosphorus sulfide

D

tetraphosphorus nonasulfide
25070-46-6

tetraphosphorus nonasulfide

E

sulfur
7704-34-9

sulfur

Conditions
ConditionsYield
In neat (no solvent) heating (dehydration at 500-550°C, 13-130 Pa, 10 min, open quartz ampoule), sealing of ampoule and heating again (1000-1050°C); mixt. of products not sepd.; (31)P-NMR spectroscopy;
phosphorus

phosphorus

sulfur
7704-34-9

sulfur

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In melt melting together P and S in a glycerine bath at 170°C;; recrystn. from CS2;;
With phosphoric acid In melt formation from P and S in the melt, with less than 1% H3PO4; stirring in a cast iron vessel;; distn. first at atm. pressure, then in vac.;;
In neat (no solvent) continuous prepn. by heating P and S at 313-318°C under CO2-atmosphere;;
sulfur
10544-50-0

sulfur

phosphorus

phosphorus

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In melt stoich. amts. of reagents are reacted in a quartz tube under vac.; recrystn. from CS2;
thionyl chloride
7719-09-7

thionyl chloride

phosphan
7803-51-2

phosphan

A

trichlorothiophosphine
3982-91-0

trichlorothiophosphine

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

C

sulfur dioxide
7446-09-5

sulfur dioxide

Conditions
ConditionsYield
In not given react. of SOCl2 with PH3;;
In not given react. of SOCl2 with PH3;;
thionyl chloride
7719-09-7

thionyl chloride

phosphan
7803-51-2

phosphan

A

phosphorus

phosphorus

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In not given react. of PH3 with SOCl2 at ambient temp.;;
phosphorous
12185-10-3

phosphorous

sulfur
7704-34-9

sulfur

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In not given
In neat (no solvent) heating P4 with S at 165°C;; extraction with CS2 or PCl3;;
In further solvent(s) slow addn. of a soln. of S in αchloronaphthalene heated to 150°C to a boiling soln. of P4 in αchloronaphthalene under CO2-atmosphere; boiling for 1 h;; filtn. and washing with CCl4;;
phosphorus
12185-10-3

phosphorus

sulfur
7704-34-9

sulfur

A

tetraphosphorus decasulfide
15857-57-5

tetraphosphorus decasulfide

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

P4S8, I
37295-14-0

P4S8, I

D

phosphorus sulfide
12037-82-0

phosphorus sulfide

E

tetraphosphorus nonasulfide
25070-46-6

tetraphosphorus nonasulfide

Conditions
ConditionsYield
In carbon disulfide vac.; several months, room temp., light; followed by (31)P NMR;
phosphorus
12185-10-3

phosphorus

sulfur
7704-34-9

sulfur

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

P4S8, II
169833-95-8

P4S8, II

P4S7, III
169833-94-7

P4S7, III

P4S7, II

P4S7, II

P4S6, α

P4S6, α

Conditions
ConditionsYield
In carbon disulfide vac.; several months, room temp., light; followed by (31)P NMR;
phosphorus
12185-10-3

phosphorus

sulfur
7704-34-9

sulfur

A

tetraphosphorus decasulfide
15857-57-5

tetraphosphorus decasulfide

B

phosphorus sulfide
1314-85-8

phosphorus sulfide

C

phosphorus sulfide
12037-82-0

phosphorus sulfide

D

tetraphosphorus nonasulfide
25070-46-6

tetraphosphorus nonasulfide

Conditions
ConditionsYield
In melt vac.; 15-79 mol% S, heating (363 K, 10-30 d); extraction (CS2), fitln., followed by (31)P NMR;
phosphan
7803-51-2

phosphan

sulfur
7704-34-9

sulfur

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In neat (no solvent) byproducts: P, H2S; react. of PH3 with S above 320°C (ratio: 2:3);;
phosphorous

phosphorous

sulfur
7704-34-9

sulfur

phosphorus sulfide
1314-85-8

phosphorus sulfide

Conditions
ConditionsYield
In neat (no solvent) heating red P with powdered S at 100°C under CO2 atmosphere or in a evacuated react.-tube;; distn. by further heating; extraction with CS2; distn. under CO2-atmosphere;;
iodine In not given formation from red P and S with I2 as catalyst;;
In neat (no solvent) formation from red P and S at 250-330°C in a stream of CO2;;
tetraphosphorus pentasulphide
15578-54-8

tetraphosphorus pentasulphide

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

phosphorus sulfide
12037-82-0

phosphorus sulfide

Conditions
ConditionsYield
In neat (no solvent) reversible react. at higher temp.;;
In not given formation from P4S5 at higher temp.;;
tetraphosphorus pentasulphide
15578-54-8

tetraphosphorus pentasulphide

triphenyl arsine sulfide
3937-40-4

triphenyl arsine sulfide

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

phosphorus sulfide
12037-82-0

phosphorus sulfide

C

γ-P4S6
189556-96-5

γ-P4S6

D

β-P4S8
169833-95-8

β-P4S8

E

α-P4S6
189556-95-4

α-P4S6

Conditions
ConditionsYield
In carbon disulfide absence of air and moisture; molar ratio P4S5:Ph3AsS=1:1, stirring for 2h; product mixt. not sepd., detd by (31)P-NMR spectroscopy;
tetraphosphorus pentasulphide
15578-54-8

tetraphosphorus pentasulphide

triphenyl arsine sulfide
3937-40-4

triphenyl arsine sulfide

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

phosphorus sulfide
12037-82-0

phosphorus sulfide

C

γ-P4S6
189556-96-5

γ-P4S6

D

α-P4S6
189556-95-4

α-P4S6

Conditions
ConditionsYield
In carbon disulfide absence of air and moisture; molar ratio P4S5:Ph3AsS=0.2-1:1, stirring for 2 h; product mixt. not sepd., detd by (31)P-NMR spectroscopy; product ratio depending on educt ratio;
tetraphosphorus pentasulphide
15578-54-8

tetraphosphorus pentasulphide

triphenyl arsine sulfide
3937-40-4

triphenyl arsine sulfide

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

phosphorus sulfide
12037-82-0

phosphorus sulfide

C

tetraphosphorus nonasulfide
25070-46-6

tetraphosphorus nonasulfide

D

β-P4S8
169833-95-8

β-P4S8

E

α-P4S6
189556-95-4

α-P4S6

Conditions
ConditionsYield
In carbon disulfide absence of air and moisture; molar ratio P4S5:Ph3AsS=2:1, stirring for 2h; product mixt. not sepd., detd by (31)P-NMR spectroscopy;
hydrogen sulfide
7783-06-4

hydrogen sulfide

tetraphenyl phosphonium chloride
2001-45-8

tetraphenyl phosphonium chloride

phosphorus trichloride
7719-12-2, 52843-90-0

phosphorus trichloride

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

tetraphenylphosphonium dichlorodithiophosphate

tetraphenylphosphonium dichlorodithiophosphate

Conditions
ConditionsYield
With α-picoline In further solvent(s) byproducts: (HNC6H8)Cl; passing dry H2S in a soln. of PCl3 in 2-methylpyridine, exotherm react., cooling of mixture in H2O-bath to 20-30°C, yellow ppt.; condensation of excess 2-methylpyridine, elution of residue with CS2 (twice), isolation of P4S3 by sepn. of solvent from eluate, washing with CH2Cl2, drying in vac.; dissoln. of solid residue in CH3CN and isolation as Ph4P-salt; elem. anal.;
hydrogen sulfide
7783-06-4

hydrogen sulfide

phosphorus trichloride
7719-12-2, 52843-90-0

phosphorus trichloride

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

phosphorus sulfide
131105-01-6

phosphorus sulfide

C

phosphorus sulfide
12037-82-0

phosphorus sulfide

tetraphosphorus pentasulphide
15578-54-8

tetraphosphorus pentasulphide

Conditions
ConditionsYield
With NaY zeolite vac. line; P-compd. condensation into zeolite, H2S condensation into PCl3/zeolite at liq. N2 temp. (ratio P:S=4:10), mixt. sealing, heating at 164°C;
hydrogen sulfide
7783-06-4

hydrogen sulfide

phosphorus trichloride
7719-12-2, 52843-90-0

phosphorus trichloride

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

phosphorus sulfide
131105-01-6

phosphorus sulfide

tetraphosphorus pentasulphide
15578-54-8

tetraphosphorus pentasulphide

Conditions
ConditionsYield
With NaY zeolite vac. line; P-compd. condensation into zeolite, H2S condensation into PCl3/zeolite at liq. N2 temp. (ratio P:S=4:3 or 4:5), mixt. sealing, heating at 100°C;
hydrogen sulfide
7783-06-4

hydrogen sulfide

phosphorus trichloride
7719-12-2, 52843-90-0

phosphorus trichloride

A

phosphorus sulfide
1314-85-8

phosphorus sulfide

B

phosphorus sulfide
12037-82-0

phosphorus sulfide

Conditions
ConditionsYield
With NaY zeolite vac. line; P-compd. condensation into zeolite, H2S condensation into PCl3/zeolite at liq. N2 temp. (ratio P:S=4:5), mixt. sealing, heating at 100°C;
phosphorus sulfide
1314-85-8

phosphorus sulfide

Ag(CH2Cl2)Al(pftb)4

Ag(CH2Cl2)Al(pftb)4

[Ag(P4S3)2][Al(pftb)4]

[Ag(P4S3)2][Al(pftb)4]

Conditions
ConditionsYield
In carbon disulfide; dichloromethane Ag(CH2Cl2)Al(pftb)4 and P4S3 in CS2-CH2Cl2 were stirred overnight at room temp.; suspn. was filtered, filtrate was concd. and stored at 0°C; elem.anal.;90%
phosphorus sulfide
1314-85-8

phosphorus sulfide

boron tribromide
10294-33-4

boron tribromide

P4S3BBr3
366837-15-2

P4S3BBr3

Conditions
ConditionsYield
In carbon disulfide (N2); P4S3 in CS2 was added to soln. of BBr3 in CS2 at room temp.; cooled to -78°C; filtered; dried in vac. at room temp.;88%
phosphorus sulfide
1314-85-8

phosphorus sulfide

[Re(1,1,1-tris(diphenylphosphanylmethyl)ethane)(CO)2]triflate
222402-52-0

[Re(1,1,1-tris(diphenylphosphanylmethyl)ethane)(CO)2]triflate

[(triphos)Re(CO)2]2(μ,η1:1-P(apical),P(basal)-P4S3](OTf)2

[(triphos)Re(CO)2]2(μ,η1:1-P(apical),P(basal)-P4S3](OTf)2

Conditions
ConditionsYield
In dichloromethane CH2Cl2 soln. of Re-complex was brought to reflux, soln. of P4S3 in CH2Cl2 was added for 20 min, refluxed for 30 min under stirring; concd. under vac., hexane was added, filtered under N2, washed with light petroleum ether, dried under N2;81%
phosphorus sulfide
1314-85-8

phosphorus sulfide

boron triiodide
13517-10-7

boron triiodide

tetraphosphorus trisulfide boron triiodide
366837-13-0

tetraphosphorus trisulfide boron triiodide

Conditions
ConditionsYield
In carbon disulfide (N2); P4S3 (1 equiv.) in CS2 was added to soln. of BI3 (1 equiv.) in CS2at room temp.; suspn. was stirred for 15 min; filtered; washed (CS2); dried in vac. at room temp.;81%
phosphorus sulfide
1314-85-8

phosphorus sulfide

copper(I) bromide
7787-70-4

copper(I) bromide

Cu7Br7*3P4S3=(P4S3)3(CuBr)7

Cu7Br7*3P4S3=(P4S3)3(CuBr)7

Conditions
ConditionsYield
In toluene; acetonitrile under N2, by Schlenk technique; CuBr soln. in MeCN layered over P4S3 in toluene for 7 d; washed with CH2Cl2/CH3CN; dried in vac.; detd. by XRD and MAS NMR; elem.anal.;80%
phosphorus sulfide
1314-85-8

phosphorus sulfide

copper(I) bromide
7787-70-4

copper(I) bromide

triethylphosphine
554-70-1

triethylphosphine

CuBr(P4S3)(PEt3)2
1339034-68-2

CuBr(P4S3)(PEt3)2

Conditions
ConditionsYield
In toluene; acetonitrile N2; Cu compd. and phosphane in MeCN added to toluene soln. of P4S3 (0.454:1.135:0.454 molar ratio), stirred for 12 h at room temp.; evapd., dissolved (toluene), crystd. (-20°C), elem. anal.;80%
phosphorus sulfide
1314-85-8

phosphorus sulfide

copper(l) chloride

copper(l) chloride

triethylphosphine
554-70-1

triethylphosphine

CuCl(P4S3)(PEt3)2
1339034-66-0

CuCl(P4S3)(PEt3)2

Conditions
ConditionsYield
In toluene; acetonitrile N2; Cu compd. and phosphane in MeCN added to toluene soln. of P4S3 (0.454:1.135:0.454 molar ratio), stirred for 12 h at room temp.; evapd., dissolved (toluene), crystd. (-20°C), elem. anal.;80%
copper(l) iodide
7681-65-4

copper(l) iodide

phosphorus sulfide
1314-85-8

phosphorus sulfide

triethylphosphine
554-70-1

triethylphosphine

CuI(P4S3)(PEt3)2
1339034-71-7

CuI(P4S3)(PEt3)2

Conditions
ConditionsYield
In toluene; acetonitrile N2; Cu compd. and phosphane in MeCN added to toluene soln. of P4S3 (0.454:1.135:0.454 molar ratio), stirred for 12 h at room temp.; evapd., dissolved (toluene), crystd. (-20°C), elem. anal.;80%
phosphorus sulfide
1314-85-8

phosphorus sulfide

tungsten pentacarbonyl tetrahydrofuran
36477-75-5

tungsten pentacarbonyl tetrahydrofuran

W(CO)5(P4S3)
1236232-10-2

W(CO)5(P4S3)

Conditions
ConditionsYield
In tetrahydrofuran under N2 by Schlenk technique; P4S3 added to soln. of W(CO)5(THF) (1.36:2.045 mol) in THF; stirred at room temp. for 20 h; evapd.; product washed (toluene, 3 times); elem. anal.;78%
phosphorus sulfide
1314-85-8

phosphorus sulfide

AgAl(hfip)4

AgAl(hfip)4

(P4S3)AgAl(hfip)4

(P4S3)AgAl(hfip)4

Conditions
ConditionsYield
In carbon disulfide AgAl(hfip)4 and P4S3 in CS2 were stirred overnight at room temp.; suspn. was filtered, filtrate was concd. and stored at -30°C; elem. anal.;77%
phosphorus sulfide
1314-85-8

phosphorus sulfide

(η5-pentamethylcyclopentadienyl)ruthenium(II)chloro[(1-diphenylarsanyl-2-diphenylphosphanyl)ethylene]

(η5-pentamethylcyclopentadienyl)ruthenium(II)chloro[(1-diphenylarsanyl-2-diphenylphosphanyl)ethylene]

sodium tetraphenyl borate
143-66-8

sodium tetraphenyl borate

(η5-pentamethylcyclopentadienyl)ruthenium(II)[(1-diphenylarsanyl-2-diphenylphosphanyl)ethylene](η1-tetraphosphorus trisulfide) tetraphenylborate
497846-12-5, 497846-20-5

(η5-pentamethylcyclopentadienyl)ruthenium(II)[(1-diphenylarsanyl-2-diphenylphosphanyl)ethylene](η1-tetraphosphorus trisulfide) tetraphenylborate

Conditions
ConditionsYield
In tetrahydrofuran byproducts: Cl(-); (Ar), Ru complex in THF added to P4S3 in THF, treated with NaBPh4, stirred at room temp. for 2 h; slowly dissolved in ethanol/light petroleum 1:1, crystd., elem. anal.;70%
phosphorus sulfide
1314-85-8

phosphorus sulfide

(η5-pentamethylcyclopentadienyl)ruthenium(II)chloro[cis-1,2-bis(diphenylphosphanyl)ethylene]
154828-19-0

(η5-pentamethylcyclopentadienyl)ruthenium(II)chloro[cis-1,2-bis(diphenylphosphanyl)ethylene]

sodium tetraphenyl borate
143-66-8

sodium tetraphenyl borate

(η5-pentamethylcyclopentadienyl)ruthenium(II)[cis-1,2-bis(diphenylphosphanyl)ethylene](η1-tetraphosphorus trisulfide) tetraphenylborate

(η5-pentamethylcyclopentadienyl)ruthenium(II)[cis-1,2-bis(diphenylphosphanyl)ethylene](η1-tetraphosphorus trisulfide) tetraphenylborate

Conditions
ConditionsYield
In tetrahydrofuran byproducts: Cl(-); (Ar), Ru complex in THF added to P4S3 in THF, treated with NaBPh4, stirred at room temp. for 2 h; slowly dissolved in ethanol/light petroleum 1:1, crystd., elem. anal.;68%
phosphorus sulfide
1314-85-8

phosphorus sulfide

bis(cyclopentadienylchromium tricarbonyl)

bis(cyclopentadienylchromium tricarbonyl)

A

[(C5H5)Cr]4(CO)9P4S3

[(C5H5)Cr]4(CO)9P4S3

B

cyclopentadienylchromiumtricarbonyl hydride
36495-37-1

cyclopentadienylchromiumtricarbonyl hydride

C

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

D

[(η5-cyclopentadienyl)Cr(CO)2]2S

[(η5-cyclopentadienyl)Cr(CO)2]2S

Conditions
ConditionsYield
In toluene N2 or Ar-atmosphere; stirring (room temp., 13 d); filtering, chromy. (SiO2, n-hexane, n-hexane / toluene = 1 : 2, n-hexane), crystn. on concg. (-28°C), recrystn. (THF / hexane, -30°C, several d); elem. anal.;A 66%
B 19%
C 2%
D 12.7%
phosphorus sulfide
1314-85-8

phosphorus sulfide

bis{tricarbonyl(η5-cyclopentadienyl)chromium}

bis{tricarbonyl(η5-cyclopentadienyl)chromium}

A

[(η5-cyclopentadienyl)Cr(CO)2]2S

[(η5-cyclopentadienyl)Cr(CO)2]2S

B

{(C5H5)4Cr4(CO)9(P4S3)}

{(C5H5)4Cr4(CO)9(P4S3)}

Conditions
ConditionsYield
In toluene 13 d at room temp.; chromy. (silica gel, toluene/hexane 7:3);A 8%
B 66%
phosphorus sulfide
1314-85-8

phosphorus sulfide

(η5-pentamethylcyclopentadienyl)ruthenium(II)chloro[bis(diphenylphosphanyl)methane]

(η5-pentamethylcyclopentadienyl)ruthenium(II)chloro[bis(diphenylphosphanyl)methane]

sodium tetraphenyl borate
143-66-8

sodium tetraphenyl borate

(η5-pentamethylcyclopentadienyl)ruthenium(II)[bis(diphenylphosphanyl)methane](η1-tetraphosphorus trisulfide) tetraphenylborate
497846-08-9, 497846-16-9

(η5-pentamethylcyclopentadienyl)ruthenium(II)[bis(diphenylphosphanyl)methane](η1-tetraphosphorus trisulfide) tetraphenylborate

Conditions
ConditionsYield
In tetrahydrofuran byproducts: Cl(-); (Ar), Ru complex in THF added to P4S3 in THF, treated with NaBPh4, stirred at room temp. for 2 h; slowly dissolved in ethanol/light petroleum 1:1, crystd., elem. anal.;65%
phosphorus sulfide
1314-85-8

phosphorus sulfide

pentamethylcyclopentadienyl(1,2-bis(diphenylphosphino)ethane)chlororuthenium(II)

pentamethylcyclopentadienyl(1,2-bis(diphenylphosphino)ethane)chlororuthenium(II)

sodium tetraphenyl borate
143-66-8

sodium tetraphenyl borate

(η5-pentamethylcyclopentadienyl)ruthenium(II)[bis(diphenylphosphanyl)ethane](η1-tetraphosphorus trisulfide) tetraphenylborate
497846-06-7, 497846-14-7

(η5-pentamethylcyclopentadienyl)ruthenium(II)[bis(diphenylphosphanyl)ethane](η1-tetraphosphorus trisulfide) tetraphenylborate

Conditions
ConditionsYield
In tetrahydrofuran byproducts: Cl(-); (Ar), Ru complex in THF added to P4S3 in THF, treated with NaBPh4, stirred at room temp. for 2 h; slowly dissolved in ethanol/light petroleum 1:1, crystd., elem. anal.;65%
phosphorus sulfide
1314-85-8

phosphorus sulfide

[CpFeCl(dppe)]
32843-51-9

[CpFeCl(dppe)]

silver trifluoromethanesulfonate
2923-28-6

silver trifluoromethanesulfonate

[(η5-C5H5)Fe(1,2-(diphenylphosphino)ethane)(η1-P(basal)-tetraphosphorus trisulfide)] triflate
1221971-68-1

[(η5-C5H5)Fe(1,2-(diphenylphosphino)ethane)(η1-P(basal)-tetraphosphorus trisulfide)] triflate

Conditions
ConditionsYield
In tetrahydrofuran; dichloromethane (N2); slurry of Fe compd., AgOTf and P4S3 in CH2Cl2/THF stirred for 4 h; mixt. filtered, filtrate evapd. under vac., residue washed with toluene and n-hexane, dried; elem. anal.;60%
phosphorus sulfide
1314-85-8

phosphorus sulfide

[CpFeCl(dppe)]
32843-51-9

[CpFeCl(dppe)]

silver trifluoromethanesulfonate
2923-28-6

silver trifluoromethanesulfonate

[((η5-C5H5)Fe(1,2-bis(diphenylphosphino)ethane))2(μ,η1:1-P(apical)-P(basal)-tetraphosphorus trisulfide)](triflate)2

[((η5-C5H5)Fe(1,2-bis(diphenylphosphino)ethane))2(μ,η1:1-P(apical)-P(basal)-tetraphosphorus trisulfide)](triflate)2

Conditions
ConditionsYield
In tetrahydrofuran; dichloromethane (N2); slurry of Fe compd., AgOTf, and P4S3 in CH2Cl2/THF stirred for 4 h; mixt. filtered, filtrate evapd. under vac., residue washed with toluene and n-hexane, dried; elem. anal.;60%
phosphorus sulfide
1314-85-8

phosphorus sulfide

bis(cyclopentadienylchromium tricarbonyl)

bis(cyclopentadienylchromium tricarbonyl)

A

[(C5H5)Cr]4(CO)9P4S3

[(C5H5)Cr]4(CO)9P4S3

B

[(CpCr(CO)2)2(μ,η(2)-P2)]

[(CpCr(CO)2)2(μ,η(2)-P2)]

C

[(η5-cyclopentadienyl)Cr(CO)2]2S

[(η5-cyclopentadienyl)Cr(CO)2]2S

D

di-η5-cyclopentadienyldichromiumtetracarbonyl

di-η5-cyclopentadienyldichromiumtetracarbonyl

Conditions
ConditionsYield
With isoprene In toluene N2 or Ar-atmosphere; stirring (room temp., 9 d); filtering, concg., chromy. (SiO2, n-hexane, n-hexane / toluene = 9 : 1, 8 : 2, 7 : 3, 1 : 1, toluene, ether), evapn.;A 58.9%
B 2.5%
C 5.3%
D 4.4%
phosphorus sulfide
1314-85-8

phosphorus sulfide

(Cr(η5-C5H5)(CO)2)2Se
91043-03-7

(Cr(η5-C5H5)(CO)2)2Se

A

(C5H5)4Cr4(CO)9(P4Se3)

(C5H5)4Cr4(CO)9(P4Se3)

B

cyclopentadienylchromiumtricarbonyl hydride
36495-37-1

cyclopentadienylchromiumtricarbonyl hydride

C

(C5H5)4Cr4(CO)8(P2Se2)

(C5H5)4Cr4(CO)8(P2Se2)

D

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

E

[(η5-cyclopentadienyl)Cr(CO)2]2S

[(η5-cyclopentadienyl)Cr(CO)2]2S

Conditions
ConditionsYield
In toluene N2-atmosphere; stirring (room temp., 6 d), filtering; chromy. (SiO2, n-hexane / toluene);A 6.4%
B 5%
C 51.5%
D 1%
E 15.5%
phosphorus sulfide
1314-85-8

phosphorus sulfide

dicarbonylcyclopentadienylbromoiron(II)

dicarbonylcyclopentadienylbromoiron(II)

silver tetrakis([2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethyl]oxy)aluminate
428441-32-1

silver tetrakis([2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethyl]oxy)aluminate

[[CpFe(CO)2]-P4S3][Al(OC(CF3)3)4]

[[CpFe(CO)2]-P4S3][Al(OC(CF3)3)4]

Conditions
ConditionsYield
Stage #1: phosphorus sulfide; silver tetrakis([2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethyl]oxy)aluminate In dichloromethane at 20℃; Inert atmosphere;
Stage #2: dicarbonylcyclopentadienylbromoiron(II) In dichloromethane for 32h; Inert atmosphere;
50%
phosphorus sulfide
1314-85-8

phosphorus sulfide

nickel(II) tetrafluoroborate hexahydrate

nickel(II) tetrafluoroborate hexahydrate

[2-((diphenylphospino)methyl)-2-methyl-1,3-propanediyl]bis[diphenylphosphine]
22031-12-5

[2-((diphenylphospino)methyl)-2-methyl-1,3-propanediyl]bis[diphenylphosphine]

[(1,1,1-tris(diphenylphosphinomethyl)ethane)Ni(η3-cyclotriphosphorus)]BF4*ethanol

[(1,1,1-tris(diphenylphosphinomethyl)ethane)Ni(η3-cyclotriphosphorus)]BF4*ethanol

Conditions
ConditionsYield
With ethanol In tetrahydrofuran; ethanol; benzene under N2, solm. of P4S3 in benzene added to soln. obtained by mixing Nisalt in ethanol and triphos in THF, refluxed for 2 h; concd. under N2, crystals filtered off, dried in vac., recrystd. from acetone and ethanol; elem. anal.;45%
sulfur
10544-50-0

sulfur

ammonium nitrate

ammonium nitrate

phosphorus sulfide
1314-85-8

phosphorus sulfide

sodiumsulfide nonahydrate

sodiumsulfide nonahydrate

A

tetrasodium hexathiodiphosphate(IV)

tetrasodium hexathiodiphosphate(IV)

B

pentaammonium 2-oxoheptathiotriphosphate (IV,III,IV) trihydrate

pentaammonium 2-oxoheptathiotriphosphate (IV,III,IV) trihydrate

Conditions
ConditionsYield
In water P4S3 was added to an aq. soln. of Na2S*9H2O and S8 under stirring (temp. increase to about 50°C); the soln. was heated at 80 °C for 45 min and H2O added; after cooling to room temp. pptn. by addn. of ethanol;; isolation of S2O6(4-): recrystn. of the ppt. from a small amt. of hot H2O; isolation of S3P7O(5-) from filtrate: addn. of EtOH, stirring for 15-20 min, decantation, repeated pptn. from aq. Ca(Ac)2/NH4NO3 soln. with EtOH; elem. anal.;;A 40%
B n/a
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
12092-47-6

di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium

phosphorus sulfide
1314-85-8

phosphorus sulfide

[2-((diphenylphospino)methyl)-2-methyl-1,3-propanediyl]bis[diphenylphosphine]
22031-12-5

[2-((diphenylphospino)methyl)-2-methyl-1,3-propanediyl]bis[diphenylphosphine]

{(triphos)Rh(P3S3)}*C6H6
87890-72-0

{(triphos)Rh(P3S3)}*C6H6

Conditions
ConditionsYield
In tetrahydrofuran; butan-1-ol; benzene N2-atmosphere; refluxing (5 h); concn. of hot soln. (crystn.);35%
In not given
In tetrahydrofuran; benzene P4S3 (2 mmol) in benzene (50 ml) was added to a mixture of triphos (2 mmol) in THF (20 ml) and {RhCl(cod)}2 (1 mmol) in THF (50 ml) under nitrogen, reflux for 1 h, addition of 40 ml warm 1-butanol; filtration, refluxing filtrate overnight;; crystals washed with ethanol and light petroleum (bp 40-70 ° C), recrystn. from benzene and CH2Cl2, elem. anal.;;35-40
phosphorus sulfide
1314-85-8

phosphorus sulfide

phosphorus sulfide
12037-82-0

phosphorus sulfide

Conditions
ConditionsYield
With I2 In carbon disulfide byproducts: PI3; react. of iodine in CS2 with P4S3;;34%
With iodine In not given byproducts: PI3; react. of P4S3 with iodine;;
With I2 In not given byproducts: PI3; react. of P4S3 with iodine;;
With S In not given
phosphorus sulfide
1314-85-8

phosphorus sulfide

di-η5-cyclopentadienyldichromiumtetracarbonyl

di-η5-cyclopentadienyldichromiumtetracarbonyl

A

cyclopentadienylchromiumtricarbonyl hydride
36495-37-1

cyclopentadienylchromiumtricarbonyl hydride

B

[(CpCr(CO)2)2(μ,η(2)-P2)]

[(CpCr(CO)2)2(μ,η(2)-P2)]

C

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

D

4Cr(2+)*4C5H5(1-)*4S(1-)=(C5H5)4Cr4(S)4

4Cr(2+)*4C5H5(1-)*4S(1-)=(C5H5)4Cr4(S)4

Conditions
ConditionsYield
In toluene N2 or Ar-atmosphere; stirring (room temp., 24 h, 60°C, 18 h); filtering, concg., chromy. (SiO2, n-hexane / toluene = 4 : 1, 3 : 1, 1 :1, toluene / ether = 1 : 1), evapn.;A 34%
B 14%
C 10%
D 30%
phosphorus sulfide
1314-85-8

phosphorus sulfide

(η5-C5H5)Fe(CO)PPh3Br

(η5-C5H5)Fe(CO)PPh3Br

silver tetrakis([2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethyl]oxy)aluminate
428441-32-1

silver tetrakis([2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethyl]oxy)aluminate

[[CpFe(PPh3)(CO)]-P4S3][Al(OC(CF3)3)4]

[[CpFe(PPh3)(CO)]-P4S3][Al(OC(CF3)3)4]

Conditions
ConditionsYield
Stage #1: phosphorus sulfide; silver tetrakis([2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethyl]oxy)aluminate In dichloromethane at 20℃; Inert atmosphere;
Stage #2: (η5-C5H5)Fe(CO)PPh3Br In dichloromethane for 28h; Inert atmosphere;
34%
cobalt(II) tetrafluoroborate hexahydrate
15684-35-2

cobalt(II) tetrafluoroborate hexahydrate

phosphorus sulfide
1314-85-8

phosphorus sulfide

[2-((diphenylphospino)methyl)-2-methyl-1,3-propanediyl]bis[diphenylphosphine]
22031-12-5

[2-((diphenylphospino)methyl)-2-methyl-1,3-propanediyl]bis[diphenylphosphine]

η3-thiadiphosphirene-(1,1,1-tris(diphenylphosphinomethyl)ethane)cobalt(II) tetrafluoroborate benzene solvate

η3-thiadiphosphirene-(1,1,1-tris(diphenylphosphinomethyl)ethane)cobalt(II) tetrafluoroborate benzene solvate

Conditions
ConditionsYield
With benzene In tetrahydrofuran; ethanol; benzene P4S3 dissolved in benzene was added to soln. of Co(BF4)2*6H2O in EtOH and ligand in THF, soln. was refluxed under N2 for 1 h; concd. under N2;30%
With benzene In ethanol; benzene under N2 atm. warm soln. P4S3 in benzene added to soln. Co(BF4)2*6H2O in ethanol and toome in benzene, soln. refluxed overnight; ethanol added, soln. concd., complex collected, washed with ethanol-benzene (1:1) and light petroleum (b.p. 40-70°C) and dried, recrystd. from CH2Cl2 and benzene; elem. anal.;
phosphorus sulfide
1314-85-8

phosphorus sulfide

(η5-1,3-C5H3(t-Bu)2)2Zr(CO)2

(η5-1,3-C5H3(t-Bu)2)2Zr(CO)2

[((C5H3tBu2)2Zr)2(μ,η1:1:1:1-P2S4)]

[((C5H3tBu2)2Zr)2(μ,η1:1:1:1-P2S4)]

Conditions
ConditionsYield
In toluene Inert atmosphere; Schlenk technique; Glovebox; Reflux;30%
phosphorus sulfide
1314-85-8

phosphorus sulfide

bis(cyclopentadienylchromium tricarbonyl)

bis(cyclopentadienylchromium tricarbonyl)

A

[(C5H5)Cr]4(CO)9P4S3

[(C5H5)Cr]4(CO)9P4S3

B

cyclopentadienylchromiumtricarbonyl hydride
36495-37-1

cyclopentadienylchromiumtricarbonyl hydride

C

[(CpCr(CO)2)2(μ,η(2)-P2)]

[(CpCr(CO)2)2(μ,η(2)-P2)]

D

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

dicarbonyl(η5-cyclopentadienyl)(cyclotriphosphanetriyl)chromium

E

4Cr(2+)*4C5H5(1-)*4S(1-)=(C5H5)4Cr4(S)4

4Cr(2+)*4C5H5(1-)*4S(1-)=(C5H5)4Cr4(S)4

Conditions
ConditionsYield
In toluene N2 or Ar-atmosphere; stirring (60°C, 3 d); filtering, concg., chromy. (SiO2, n-hexane, n-hexane / toluene = 9 : 1, 8 : 2, 7 : 3, 1 : 1, toluene, ether), evapn.;A 22.2%
B 3%
C 1%
D 0.4%
E 6.8%

1314-85-8Relevant articles and documents

Adduct compounds (MCl5)2(β-P4Ch 4) with M = Nb, Ta and Ch = S, Se

Hoppe, Diana,Pfitzner, Arno

, p. 58 - 62 (2009)

Adduct compounds of the general composition (MCl5) 2(β-P4Ch4), M = Nb, Ta and Ch = S, Se, were obtained from solutions of M2Cl10 and P 4Ch3 in CS2 / n-hexan

Phosphorus chalcogen molecules as complex ligands - Reactions with NbCl5

Nowottnick, Heike,Stumpf, Klaus,Blachnik, Roger,Reuter, Hans

, p. 693 - 697 (1999)

The reaction of P4E3 (E = S, Se) with NbCl5 yields [β-P4S4(NbCl5)2] and [P4Se3(NbCl5)]. [β-P4S4(NbCl5)2] crystallizes in the monoclinic space group P21/n with the lattice parameters a = 6.226(1), b = 12.971(2), c = 26.380(2) A, β = 93.7(1) (Z = 4). In this compound a sulfur atom is introduced into the basal P3-ring and the resulting β-P4S4 is central unit of the complex. [P4Se3(NbCl5)] crystallizes in the same space group type with the lattice parameters a = 11.939(1), b = 18.603(2), c = 12.763(4) A, β= 90.16(2)° (Z = 8). In both compounds the ligands are coordinated to basal phosphorus atoms.

Synthesis of cationic R2P5+ cages and subsequent chalcogenation reactions

Holthausen, Michael H.,Hepp, Alexander,Weigand, Jan J.

supporting information, p. 9895 - 9907 (2013/08/23)

Cationic R2P5+ cage compounds (1 +) have been synthesized by the stoichiometric reaction of R 2PCl, GaCl3 and P4. The reaction conditions depend on the substituent R. Alkyl-substituted derivatives (1 a-1 d[GaCl 4]) are best synthesized under solvent-free conditions, whereas aryl-substituted derivatives (1 e-1 h[GaCl4]) are formed in C 6H5F. All compounds have been prepared on a multi-gram scale in good to excellent yields and have been fully characterized with an emphasis on 31P NMR spectroscopy in solution and single-crystal structure determination. Subsequent chalcogenation reactions of cations R 2P5+ (1 a+, 1 e+) and trication Ph6P73+ (33+) with elemental sulfur (α-S8) or grey selenium (Segrey) yielded a series of unique polyphosphorus-chalcogen cations (4 a+, 4 e+, 5 a+, 62+ and 72+ Copyright

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