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1072-53-3

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  • Ethylene sulfate CAS 1072-53-3 Glycol sulfite 1,3,2-Dioxathiolane 2,2-dioxide CAS 1072-53-3

    Cas No: 1072-53-3

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1072-53-3 Usage

Chemical Properties

White Solid

Uses

Different sources of media describe the Uses of 1072-53-3 differently. You can refer to the following data:
1. 1,3,2-Dioxathiolane 2,2-Dioxide is an alkylating agent with carcinogenic activty.
2. 1,3,2-Dioxathiolane 2,2-dioxide may be employed in the preparation of imidazolidinium salts.

Check Digit Verification of cas no

The CAS Registry Mumber 1072-53-3 includes 7 digits separated into 3 groups by hyphens. The first part of the number,starting from the left, has 4 digits, 1,0,7 and 2 respectively; the second part has 2 digits, 5 and 3 respectively.
Calculate Digit Verification of CAS Registry Number 1072-53:
(6*1)+(5*0)+(4*7)+(3*2)+(2*5)+(1*3)=53
53 % 10 = 3
So 1072-53-3 is a valid CAS Registry Number.
InChI:InChI=1/C2H4O4S/c3-7(4)5-1-2-6-7/h1-2H2

1072-53-3 Well-known Company Product Price

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  • TCI America

  • (D2830)  1,3,2-Dioxathiolane 2,2-Dioxide  >98.0%(GC)

  • 1072-53-3

  • 5g

  • 790.00CNY

  • Detail
  • TCI America

  • (D2830)  1,3,2-Dioxathiolane 2,2-Dioxide  >98.0%(GC)

  • 1072-53-3

  • 25g

  • 2,890.00CNY

  • Detail
  • Aldrich

  • (471690)  1,3,2-Dioxathiolane2,2-dioxide  98%

  • 1072-53-3

  • 471690-5G

  • 993.33CNY

  • Detail

1072-53-3SDS

SAFETY DATA SHEETS

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

Version: 1.0

Creation Date: Aug 10, 2017

Revision Date: Aug 10, 2017

1.Identification

1.1 GHS Product identifier

Product name 1,3,2-Dioxathiolane 2,2-dioxide

1.2 Other means of identification

Product number -
Other names ETHYLENESULFATE

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:1072-53-3 SDS

1072-53-3Synthetic route

oxirane
75-21-8

oxirane

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With cerium(IV) oxide; iron(III) chloride; sulfur dioxide; antimony(III) chloride at 140℃; under 45004.5 Torr; for 2h; Pressure; Temperature; Inert atmosphere; Autoclave;97.8%
With aminosulfonic acid; acetic anhydride at -10 - 20℃; for 24h; Autoclave;73.22%
ethylene glycol
107-21-1

ethylene glycol

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With fluorosulfonyl fluoride; N,N,N,N,-tetramethylethylenediamine In acetonitrile at 60℃; for 36h; Reagent/catalyst; Solvent; Temperature;96.5%
Stage #1: ethylene glycol With fluorosulfonyl fluoride; sodium sulfate; tetra(n-butyl)ammonium hydrogensulfate; sodium hydroxide In tert-butyl methyl ether at 5 - 10℃; for 1h; Autoclave;
Stage #2: With 15-crown-5; 18-crown-6 ether In dichloromethane Solvent; Reagent/catalyst; Temperature;
81.8%
With potassium hydroxide; sulfuryl dichloride; silica gel 1.) reflux; 2.) rt., 3 h; Yield given. Multistep reaction;
Stage #1: ethylene glycol With potassium hydroxide In 5,5-dimethyl-1,3-cyclohexadiene at 130 - 140℃; for 20h;
Stage #2: With fluorosulfonyl fluoride In acetonitrile at -15 - -5℃; for 1h; Temperature; Reagent/catalyst; Solvent; Sealed tube; Inert atmosphere;
106.3 g
With sulfuryl dichloride In chloroform at 5 - 60℃; for 3h;375 g
ethylene sulfite
3741-38-6

ethylene sulfite

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With manganese(IV) oxide In water at 5℃; for 0.75h; Reagent/catalyst; Temperature;95.84%
With sodium hydrogencarbonate; iron(II) sulfate In dichloromethane pH=7 - 8; Concentration;90.66%
With ruthenium trichloride; calcium hypochlorite at 15℃;83%
ethene
74-85-1

ethene

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With PhI(1+)OSO2O(1-) In dichloromethane at 15℃; for 0.3h;85%
With μ-oxodiphenyldiiodine(III) sulfate; phenyliodine(III) sulfate Yield given;
[1,3]-dioxolan-2-one
96-49-1

[1,3]-dioxolan-2-one

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With carbon dioxide; sulfur trioxide at 25 - 65℃; for 8h; Inert atmosphere;76%
thionyl chloride
7719-09-7

thionyl chloride

ethylene glycol
107-21-1

ethylene glycol

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
Stage #1: thionyl chloride; ethylene glycol at 25 - 30℃; for 3h; Inert atmosphere;
Stage #2: With sodium hypochlorite; ruthenium(III) chloride trihydrate at 0 - 10℃; for 3h; pH=7-8; Concentration; Temperature;
74%
C2H5ClO3S

C2H5ClO3S

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With sodium periodate; ruthenium(III) chloride trihydrate In water; acetonitrile for 0.25h; Cooling with ice; Inert atmosphere;70%
ethylene dibromide
106-93-4

ethylene dibromide

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With silver sulfate; xylene
With silver sulfate In xylene
ethylene sulfite
3741-38-6

ethylene sulfite

ruthenium (IV) oxide dihydrate

ruthenium (IV) oxide dihydrate

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
With sodium hypochlorite In dichloromethane; isopropyl alcohol
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Conditions
ConditionsYield
Stage #1: potassium ethyleneglycolate With sulfuryl dichloride In dichloromethane at -10 - 10℃; for 2h; Inert atmosphere;
Stage #2: With 18-crown-6 ether In toluene at 20℃; for 1h; Reagent/catalyst; Solvent;
37.9 g
ethane
74-84-0

ethane

A

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

B

ethane-1,2-diyl bis(hydrogen sulfate)
6914-91-6

ethane-1,2-diyl bis(hydrogen sulfate)

Conditions
ConditionsYield
With fuming sulphuric acid; iodine at 90℃; under 22502.3 Torr; for 2h; Catalytic behavior; Reagent/catalyst; Temperature; Autoclave;
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

tert-butyl cinnamate
14990-09-1

tert-butyl cinnamate

C12H20NSi(1-)*Li(1+)

C12H20NSi(1-)*Li(1+)

(-)-tert-butyl (2S,3R)-1-benzyl-2-phenylpyrrolidine-3-carboxylate
1394979-11-3

(-)-tert-butyl (2S,3R)-1-benzyl-2-phenylpyrrolidine-3-carboxylate

Conditions
ConditionsYield
Stage #1: C12H20NSi(1-)*Li(1+) With (1S,2S)-1,2-dimethoxy-1,2-diphenylethane In toluene at -78℃; for 0.583333h;
Stage #2: tert-butyl cinnamate In toluene at -78℃; for 1.63h;
Stage #3: ethyleneglycol sulfate enantioselective reaction; Further stages;
97%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2-methyl-acrylic acid 3-dimethylamino-propyl amide
5205-93-6

2-methyl-acrylic acid 3-dimethylamino-propyl amide

2-((3-methacrylamidopropyl)dimethylammonio)ethyl sulfate

2-((3-methacrylamidopropyl)dimethylammonio)ethyl sulfate

Conditions
ConditionsYield
With nitrobenzene In acetonitrile at 50℃; for 24h; Schlenk technique; Inert atmosphere;95.6%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

difluoromethyl phenyl sulfone
1535-65-5

difluoromethyl phenyl sulfone

3,3-difluoro-3-(phenylsulfonyl)propan-1-ol

3,3-difluoro-3-(phenylsulfonyl)propan-1-ol

Conditions
ConditionsYield
With N,N,N,N,N,N-hexamethylphosphoric triamide; sulfuric acid; lithium hexamethyldisilazane In tetrahydrofuran; water at 20℃; for 2h;94%
Stage #1: ethyleneglycol sulfate; difluoromethyl phenyl sulfone With N,N,N,N,N,N-hexamethylphosphoric triamide; lithium hexamethyldisilazane In tetrahydrofuran at -78 - 20℃; for 3.5h; Inert atmosphere;
Stage #2: With sulfuric acid In tetrahydrofuran at 60℃;
90%
6-methylbenzo[b]thiophene
16587-47-6

6-methylbenzo[b]thiophene

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2-(6-methyl-benzo[b]thiophen-2-yl)-ethanol
873692-99-0

2-(6-methyl-benzo[b]thiophen-2-yl)-ethanol

Conditions
ConditionsYield
Stage #1: 6-methylbenzo[b]thiophene With n-butyllithium In tetrahydrofuran; hexanes at -60℃; for 0.75h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; hexanes at -60 - 20℃;
Stage #3: With acetyl chloride In methanol at 0 - 20℃; for 4.25h;
89%
1-methyl-1H-imidazole
616-47-7

1-methyl-1H-imidazole

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

lithium diphenylphosphide
65567-06-8, 4541-02-0

lithium diphenylphosphide

2-(2-(diphenylphosphino)ethyl)-1-methyl-1H-imidazol

2-(2-(diphenylphosphino)ethyl)-1-methyl-1H-imidazol

Conditions
ConditionsYield
Stage #1: 1-methyl-1H-imidazole With n-butyllithium In tetrahydrofuran; hexane at -78 - 60℃; Inert atmosphere;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; hexane at -78 - 0℃; Inert atmosphere;
Stage #3: lithium diphenylphosphide In tetrahydrofuran; hexane at 0℃; Inert atmosphere; Reflux;
89%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2-fluoro-3-iodopyridine
113975-22-7

2-fluoro-3-iodopyridine

2-(2-fluoro-4-iodopyridin-3-yl)ethane-1-ol
1620011-25-7

2-(2-fluoro-4-iodopyridin-3-yl)ethane-1-ol

Conditions
ConditionsYield
Stage #1: 2-fluoro-3-iodopyridine With lithium diisopropyl amide In tetrahydrofuran; n-heptane at -78℃; for 1.5h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; n-heptane at -78 - 20℃; for 2.33333h;
Stage #3: With hydrogenchloride In tetrahydrofuran; n-heptane; water at 0 - 20℃; for 3h;
87%
Stage #1: 2-fluoro-3-iodopyridine With lithium diisopropyl amide In tetrahydrofuran; n-heptane; ethylbenzene at -78℃; for 1.5h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; n-heptane; ethylbenzene at -78 - 30℃; for 2.67h;
Stage #3: With hydrogenchloride; water In tetrahydrofuran; n-heptane; ethylbenzene at 0 - 30℃; for 3h;
87%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2-fluoro-4-iodopyridine
22282-70-8

2-fluoro-4-iodopyridine

2-(2-fluoro-4-iodopyridin-3-yl)ethane-1-ol
1620011-25-7

2-(2-fluoro-4-iodopyridin-3-yl)ethane-1-ol

Conditions
ConditionsYield
Stage #1: 2-fluoro-4-iodopyridine With lithium diisopropyl amide In tetrahydrofuran; n-heptane; ethylbenzene at -78℃; for 1.5h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; n-heptane; ethylbenzene at -78 - 20℃; for 2.66667h;
Stage #3: With hydrogenchloride In tetrahydrofuran; n-heptane; ethylbenzene; water at 0 - 20℃; for 3h;
87%
Stage #1: 2-fluoro-4-iodopyridine With lithium diisopropyl amide In tetrahydrofuran at -65℃; for 1.5h; Inert atmosphere;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran at -65 - 20℃; Inert atmosphere;
86.2%
Stage #1: 2-fluoro-4-iodopyridine With lithium diisopropyl amide In tetrahydrofuran; n-heptane; ethylbenzene at -78℃; for 1.5h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; n-heptane; ethylbenzene at -78 - 20℃; for 2.67h;
1950 mg
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2,2-bis((decyloxy)methyl)propane-1,3-diol
1191028-34-8

2,2-bis((decyloxy)methyl)propane-1,3-diol

disodium 5,5-bis(decyloxymethyl)-3,7-dioxa-1,9-nonadiyl disulfate

disodium 5,5-bis(decyloxymethyl)-3,7-dioxa-1,9-nonadiyl disulfate

Conditions
ConditionsYield
Stage #1: 2,2-bis((decyloxy)methyl)propane-1,3-diol With sodium hydride In tetrahydrofuran; mineral oil for 0.5h; Cooling with ice;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; mineral oil at 20℃; for 26h;
86%
Stage #1: 2,2-bis((decyloxy)methyl)propane-1,3-diol With sodium hydride In tetrahydrofuran; mineral oil for 0.5h; Cooling with ice;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; mineral oil for 24.33h;
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

1-bromo-4-(2-bromo-1,1,2,2-tetrafluoroethoxy)benzene
113939-45-0

1-bromo-4-(2-bromo-1,1,2,2-tetrafluoroethoxy)benzene

4-(4-bromophenoxy)-3,3,4,4-tetrafluorobutan-1-ol

4-(4-bromophenoxy)-3,3,4,4-tetrafluorobutan-1-ol

Conditions
ConditionsYield
Stage #1: 1-bromo-4-(2-bromo-1,1,2,2-tetrafluoroethoxy)benzene With TurboGrignard In tetrahydrofuran at -78℃; Inert atmosphere; Schlenk technique;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran at -78 - 20℃; for 3h; Inert atmosphere; Schlenk technique;
Stage #3: With sulfuric acid In water Inert atmosphere; Schlenk technique; Reflux;
86%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

8-cyclosporin

8-cyclosporin

C64H114N11O17S(1-)*Na(1+)

C64H114N11O17S(1-)*Na(1+)

Conditions
ConditionsYield
With sodium hydride In tetrahydrofuran at 30℃; for 2h;85%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

1-methyl-2-((trimethylsilyl)methyl)-1H-imidazole
91631-71-9

1-methyl-2-((trimethylsilyl)methyl)-1H-imidazole

lithium diphenylphosphide
65567-06-8, 4541-02-0

lithium diphenylphosphide

2-(2-(diphenylphosphino)ethyl)-1-methyl-1H-imidazol

2-(2-(diphenylphosphino)ethyl)-1-methyl-1H-imidazol

Conditions
ConditionsYield
Stage #1: ethyleneglycol sulfate; 1-methyl-2-[(trimethylsilyl)methyl]-1H-imidazole In tetrahydrofuran at -78 - 100℃; for 6h;
Stage #2: lithium diphenylphosphide at -78℃; Reflux;
85%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

(3S)-4-(4,6-dichloropyrimidin-2-yl)-3-methylmorpholine
1333108-98-7

(3S)-4-(4,6-dichloropyrimidin-2-yl)-3-methylmorpholine

2-{4,6-dichloro-2-[(3S)-3-methylmorpholin-4-yl]pyrimidin-5-yl}ethanol

2-{4,6-dichloro-2-[(3S)-3-methylmorpholin-4-yl]pyrimidin-5-yl}ethanol

Conditions
ConditionsYield
Stage #1: (3S)-4-(4,6-dichloropyrimidin-2-yl)-3-methylmorpholine With n-butyllithium In tetrahydrofuran at -78℃; for 0.5h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran for 0.5h;
Stage #3: With hydrogenchloride In tetrahydrofuran; water at 40℃; for 22h;
85%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

benzyl N-[2-[2-(cyanomethyl)phenoxy]ethyl]-N-methylcarbamate

benzyl N-[2-[2-(cyanomethyl)phenoxy]ethyl]-N-methylcarbamate

benzyl N-[2-[2-(1-cyanocyclopropyl)phenoxy]ethyl]-N-methylcarbamate

benzyl N-[2-[2-(1-cyanocyclopropyl)phenoxy]ethyl]-N-methylcarbamate

Conditions
ConditionsYield
Stage #1: benzyl N-[2-[2-(cyanomethyl)phenoxy]ethyl]-N-methylcarbamate With sodium hydroxide In dimethyl sulfoxide at 20 - 25℃; for 0.166667h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; dimethyl sulfoxide at 20 - 25℃; for 16h;
84.6%
4,6-dichloro-2-(morpholine-4-yl)pyrimidine
10397-13-4

4,6-dichloro-2-(morpholine-4-yl)pyrimidine

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2-[4,6-dichloro-2-(morpholin-4-yl)pyrimidin-5-yl]ethanol

2-[4,6-dichloro-2-(morpholin-4-yl)pyrimidin-5-yl]ethanol

Conditions
ConditionsYield
Stage #1: 4,6-dichloro-2-(morpholine-4-yl)pyrimidine With n-butyllithium In tetrahydrofuran; hexane at -65℃; for 0.5h; Inert atmosphere;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; hexane at -65℃; for 1.5h;
Stage #3: With hydrogenchloride In tetrahydrofuran; hexane; water at 20℃; for 18h;
84%
Stage #1: 4,6-dichloro-2-(morpholine-4-yl)pyrimidine With n-butyllithium In tetrahydrofuran at -78℃; for 0.5h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran for 0.666667h;
Stage #3: With hydrogenchloride In tetrahydrofuran; water at 20 - 40℃; for 22h;
42%
2,2-bis((dodecyloxy)methyl)propane-1,3-diol

2,2-bis((dodecyloxy)methyl)propane-1,3-diol

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

disodium 5,5-bis(dodecyloxymethyl)-3,7-dioxa-1,9-nonadiyl disulfate

disodium 5,5-bis(dodecyloxymethyl)-3,7-dioxa-1,9-nonadiyl disulfate

Conditions
ConditionsYield
Stage #1: 2,2-bis((dodecyloxy)methyl)propane-1,3-diol With sodium hydride In tetrahydrofuran; mineral oil for 0.5h; Cooling with ice;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; mineral oil at 20℃;
83.3%
Stage #1: 2,2-bis((dodecyloxy)methyl)propane-1,3-diol With sodium hydride In tetrahydrofuran; mineral oil for 0.5h; Cooling with ice;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; mineral oil at 20℃; for 21h;
83%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

tert-butyl cinnamate
14990-09-1

tert-butyl cinnamate

Lithium N-benzyl-N-(trimethylsilyl)amide
113709-50-5

Lithium N-benzyl-N-(trimethylsilyl)amide

(-)-tert-butyl (2S,3R)-1-benzyl-2-phenylazetidine-3-carboxylate
1394979-19-1

(-)-tert-butyl (2S,3R)-1-benzyl-2-phenylazetidine-3-carboxylate

Conditions
ConditionsYield
Stage #1: Lithium N-benzyl-N-(trimethylsilyl)amide With (1S,2S)-1,2-dimethoxy-1,2-diphenylethane In toluene at -78℃; for 0.583333h;
Stage #2: tert-butyl cinnamate In toluene at -78℃; for 1.63h;
Stage #3: ethyleneglycol sulfate enantioselective reaction; Further stages;
82%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

(μ-1,3-propanedithiolate)Fe2(CO)4[μ-3-(Ph2P)2NC5H4N]

(μ-1,3-propanedithiolate)Fe2(CO)4[μ-3-(Ph2P)2NC5H4N]

(μ-1,3-propanedithiolate)Fe2(CO)4[μ-3-(Ph2P)2NC5H4N((CH2)2OSO3)]

(μ-1,3-propanedithiolate)Fe2(CO)4[μ-3-(Ph2P)2NC5H4N((CH2)2OSO3)]

Conditions
ConditionsYield
In acetonitrile for 8h; Inert atmosphere; Schlenk technique; Reflux;81%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

N,N-dibenzylamino-acetonitrile
51643-96-0

N,N-dibenzylamino-acetonitrile

1-<(dibenzyl)amino>cyclopropanecarbonitrile
137360-51-1

1-<(dibenzyl)amino>cyclopropanecarbonitrile

Conditions
ConditionsYield
With N,N,N,N,N,N-hexamethylphosphoric triamide; lithium diisopropyl amide In tetrahydrofuran at -70℃;80%
With N,N,N,N,N,N-hexamethylphosphoric triamide; lithium diisopropyl amide In tetrahydrofuran at -70℃; for 1.5h; Product distribution; further dielectophiles; access to cyclopropane aminonitriles;
With N,N,N,N,N,N-hexamethylphosphoric triamide; lithium diisopropyl amide In tetrahydrofuran at -70℃; for 1.5h; Yield given;
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

(2S)-2-(6-methoxy(2-naphthyl))propanoic acid
22204-53-1

(2S)-2-(6-methoxy(2-naphthyl))propanoic acid

(S)-naproxen ethyl sulfate potassium salt

(S)-naproxen ethyl sulfate potassium salt

Conditions
ConditionsYield
With potassium tert-butylate In isopropyl alcohol at 45℃; for 0.166667h;80%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

bis(2-phenylpyridinato-N,C2)-mono(4-[hydroxymethyl]-2-pyridine carboxylato-N,O)iridium(III)

bis(2-phenylpyridinato-N,C2)-mono(4-[hydroxymethyl]-2-pyridine carboxylato-N,O)iridium(III)

tetrabutyl-ammonium chloride
1112-67-0

tetrabutyl-ammonium chloride

tetra-n-butylammonium bis(2-phenylpyridinato-N,C2)-mono(4-[sulfatoethyloxymethyl]-2-pyridinecarboxylato-N,O)iridium(III)
1119493-11-6

tetra-n-butylammonium bis(2-phenylpyridinato-N,C2)-mono(4-[sulfatoethyloxymethyl]-2-pyridinecarboxylato-N,O)iridium(III)

Conditions
ConditionsYield
With NaH In N,N-dimethyl-formamide (N2, in the absence of light); a soln. of Ir complex stirred at 0°C for 30 min, NaH added, stirred at room temp. for 16 h, (CH2O)2SO2 added, stirred for 12 h; concd., pptd. in Et2O, dissolved in CH2Cl2, added to an aq. soln. of N(C4H9)4Cl, stirred for 16 h, the org. layer sepd., washed (H2O), dried (MgSO4), concd., pptd. in Et2O; elem. anal.;80%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

methyl 2-(pyrimidin-5-yl)acetate

methyl 2-(pyrimidin-5-yl)acetate

methyl 1-(pyrimidin-5- yl)cyclopropane-1-carboxylate

methyl 1-(pyrimidin-5- yl)cyclopropane-1-carboxylate

Conditions
ConditionsYield
Stage #1: methyl 2-(pyrimidin-5-yl)acetate With lithium hexamethyldisilazane In tetrahydrofuran at -70℃; for 1h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran at -70 - -20℃; for 1.5h;
Stage #3: With lithium hexamethyldisilazane In tetrahydrofuran at -72 - 20℃; for 15h;
80%
thiophene
188290-36-0

thiophene

ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

2-thiophenethanol
5402-55-1

2-thiophenethanol

Conditions
ConditionsYield
Stage #1: thiophene With n-butyllithium In tetrahydrofuran; hexane at -78℃;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; hexane at -78 - 20℃;
Stage #3: With sulfuric acid In tetrahydrofuran; hexane for 3h; Heating; Further stages.;
79%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

Benzo[b]thiophene
95-15-8

Benzo[b]thiophene

2-(β-Hydroxyethyl)-benzothiophene
30962-69-7

2-(β-Hydroxyethyl)-benzothiophene

Conditions
ConditionsYield
Stage #1: Benzo[b]thiophene In tetrahydrofuran; hexanes at -50 - -40℃; for 0.75h;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran; hexanes at -40 - 20℃;
Stage #3: With acetyl chloride In methanol at 20℃; for 4.25h;
79%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

cyclopentylacetic acid methyl ester
2723-38-8

cyclopentylacetic acid methyl ester

3-cyclopentyldihydrofuran-2(3H)-one

3-cyclopentyldihydrofuran-2(3H)-one

Conditions
ConditionsYield
Stage #1: cyclopentylacetic acid methyl ester With lithium diisopropyl amide In tetrahydrofuran at -78℃;
Stage #2: ethyleneglycol sulfate In tetrahydrofuran at -78 - 20℃; for 5h;
Stage #3: With sulfuric acid In toluene Reflux;
79%
ethyleneglycol sulfate
1072-53-3

ethyleneglycol sulfate

di-isopropylphosphine
20491-53-6

di-isopropylphosphine

diphenylphosphane
829-85-6

diphenylphosphane

(CH(CH3)2)2PCH2CH2P(C6H5)2
262359-83-1

(CH(CH3)2)2PCH2CH2P(C6H5)2

Conditions
ConditionsYield
Multistep reaction;76%

1072-53-3Relevant articles and documents

Ham

, p. 864 (1960)

-

Kaiser et al.

, p. 602 (1963)

-

-

Baker,Field

, p. 86,87 (1932)

-

-

Lipkin,Layloff

, p. 450,451 (1970)

-

Preparation method of ethylene sulfate derivative

-

Paragraph 0027-0028; 0029-0030; 0031-0032; 0035-0040, (2021/01/25)

The invention belongs to the technical field of organic synthetic chemistry, and particularly relates to a preparation method of an ethylene sulfate derivative, which comprises the following steps: ina mixed solvent composed of an organic solvent and water, in the presence of alkali and quaternary ammonium salt, by using ruthenium trichloride as a catalyst, reacting to obtain the ethylene sulfatederivative. The ethylene sulfite derivative shown in the general formula A and trichloroisocyanuric acid shown in the formula TCCA are subjected to an oxidation reaction to obtain the ethylene sulfate derivative, and the reaction route is as follows: R1 to R4 are independently a hydrogen atom or an alkyl group of C1-3; the ethylene sulfate derivative is synthesized with high efficiency and low cost, and the yield and purity of the product are improved.

Synthesis process of ethylene sulfate

-

Paragraph 0019; 0021-0022; 0024-0025; 0027-0028; 0030-0031, (2021/02/20)

The invention discloses a synthesis process of ethylene sulfate. The synthesis process comprises the following steps: dissolving ethylene glycol in an organic solvent, dropwisely adding thionyl chloride, reacting at 5-10 DEG C for 1-1.5 hours while keeping the temperature, adding a sodium carbonate solution to regulate the pH value to 7-8, and standing to stratify to obtain an ethylene sulfite-containing mixed solution; adding a catalyst into the mixed solution containing ethylene sulfite, dropwise adding a 70% tert-butyl hydroperoxide aqueous solution for 0.5-1 hour, reacting at 30-40 DEG C for 1-3 hours after dropwise adding, then adding a sodium sulfite solution, standing for layering, carrying out aqueous phase extraction, combining organic phases, carrying out reduced pressure concentration, and recrystallizing to obtain ethylene sulfate. The mixed solution containing the ethylene sulfite is directly subjected to oxidation reaction, so that the technological process is simplified;70% tert-butyl hydroperoxide aqueous solution and copper chloride are adopted, so that the cost is further reduced; and the obtained ethylene sulfate has high yield and purity.

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