ChemicalBook CAS DataBase List Bis(trimethylsilyl)sulfate

Bis(trimethylsilyl)sulfate synthesis

13synthesis methods

Product Name:Bis(trimethylsilyl)sulfate
CAS Number:18306-29-1
Molecular formula:C6H18O4SSi2
Molecular Weight:242.44

107-46-0 Synthesis

107-46-0
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$10.00/10g

18306-29-1
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$13.00/5g

Yield:18306-29-1 37.59%

Reaction Conditions:

with sulfuric acid in toluene at 100; for 3 h;

Steps:

1.1
(1)In a four-neck bottle with a reflux device,The input contains hexamethyldisiloxane (silicon ether) (25.0g pure,About 0.1539 mol) of toluene azeotrope (containing about 30% by weight of silyl ether),Rectification and water separation at a temperature of 100 ° C,Toluene is refluxed into the system,When no water is distilled off,15.0 g of concentrated sulfuric acid (concentration 98.5%, about 0.1506 mol) was added dropwise.Continue to carry out reactive distillation to separate water,The toluene was refluxed into the system.After refluxing for 3 hours,When no water is distilled off,GC detection reaction solution,When the silyl ether residue is Stop the reaction,Allow to cool down to room temperature,At the same time, the concentration of bis(trimethylsilyl) sulfate was calculated to be about 37.59 wt%.About 0.1491 mol.

References:

Shangyu Xin He Cheng Biochemical Co., Ltd.;Zhejiang Xinhecheng Pharmaceutical Co., Ltd.;Liu Xianghong;Lv Guofeng;Tian Jinjin;Qiao Shengchao;Hang Jiao;Chen Kai CN108864172, 2018, A Location in patent:Paragraph 0070-0071

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