Chloromethyl chlorosulfate synthesis
- Product Name:Chloromethyl chlorosulfate
- CAS Number:49715-04-0
- Molecular formula:CH2Cl2O3S
- Molecular Weight:165
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Yield:49715-04-0 85% ，92975-18-3 12%
Reaction Conditions:
with sulfuric acid;boron tribromide at 20 - 30; for 4 h;Temperature;
Steps:
2.1; 2.2 Example 2A method for preparing methyl dichlorosulfonate includes the following steps:
(1) Slowly add fuming sulfuric acid with a concentration of 65% in 1-2 hours at 10-20°C.17g of boron tribromide catalyst in dichloromethane,Control reaction temperature is maintained at 20-30 ° C, the reaction time is 4h; where dichloromethane is 1mol, 84.93g; fuming sulfuric acid is 2.5mol, 307.92g;(2) After the reaction is completed, the aqueous sodium bicarbonate solution is slowly added to the reaction system to neutralize until the pH of the solution is 7-8.The mixture was allowed to stand for stratification, and the upper organic layer was taken and dried over anhydrous sodium sulfate. After filtration, 229 g of the main product, methyl dichlorosulfonate and the by-product chloromethyl chlorosulfonate were mixed, and the main product was methyl dichlorosulfone. The yield of the ester is 85%;The yield of by-product chloromethylchlorosulfonate was 12%.
References:
He Xia Chemical (Taicang) Co., Ltd.;Bang Tianshenyi;Bang Tianzhizi;Wei Wenjun;Tang Chengjian;Shi Xinghui;Wang Zhengguo CN107986995, 2018, A Location in patent:Paragraph 0011; 0024-0039
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49715-04-0
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49715-04-0
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49715-04-0
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