Synthesis
Chloromethylsulfonyl chloride is synthesized as follows: add Na2SO3252g, 500g of water, 504g of methylene chloride, I1.25g of cetyltrimethylammonium chloride to 2000ml of the reactor with a pressure and temperature detecting device, warm up to 0.2MPa pressure in the reactor and keep pressure to react for 3hr, stop the reaction, cool down, unload the reactor and remove the water and unreacted solvent by distillation. Unreacted solvent was removed by distillation and dried to obtain the product I260 g. Yield: 95%.
The above synthesized product I was added to 2000 ml reaction bottle with thermometer, drying and distillation device, add methanol 260g, triethylamine 1.04g, slowly raise the temperature to T = 40 , maintain the temperature, in 30min, through the chlorine gas 13g, keep warm to react 3.5hr, the end of the reaction. The solvent was removed by distillation. Obtained crude product, at a temperature of T = 70-80 , vacuum degree of 0.08-0.1MPa conditions, distillation, the product 240g. 85% yield.
