乙硫醇氯化法合成乙烷磺酰胺

Preparation of Ethane Sulphonamide by Chlorination of Ethyl Mercaptan

控制料比n(乙硫醇 )∶n (水 )∶n (氯气 ) =1∶(3～ 4)∶3 15 ,前期氯化温度不超过 5℃ ,中后期氯化温度不超过 2 0℃ ,原料乙硫醇、水和氯气反应生成中间体乙烷磺酰氯 ;控制胺化温度不超过30℃ ,乙烷磺酰氯与氨同时投入四氢呋喃 -氨介质中反应 ,胺化料比n(乙烷磺酰氯 )∶n(氨 ) =1∶(2 .6～ 3.0 ) ,m(乙烷磺酰氯 )∶m (四氢呋喃 ) =43∶10 0 ,过滤滤除副产品氯化铵 ,常压蒸除四氢呋喃 ,得到乙烷磺酰胺粗品 ,然后用乙酸乙酯重结晶 ,活性炭脱色 ,冷却 ,过滤结晶得到产品乙烷磺酰胺 ,w (乙烷磺酰胺 )≥ 99% ,以乙硫醇计总收率≥ 85 %。

The intermediate compound ethanesulfonyl chloride was prepared by the reaction of ethyl mercaptan,water and chlorine,controlling the material proportion n(EtSH)∶n(H 2O)∶n(C1 2)=1∶(3～4)∶3.15 and the chlorination temperature not more than 5 ℃ in the earlier period and not more than 20 ℃ in the middle and later periods.Crude ethanesulphonamide was obtained by the reaction of ethanesulfonyl chloride and ammonia added simultaneously to the media tetrahydrofuran-ammonia,controlling the materials proportion n(EtSO 2Cl)∶n(NH 3)=1∶(2.6～3.0),w(EtSO 2C1)∶w(THF)=43∶100 and the ammoniation temperature not more than 30 ℃,filtering out the by-product ammonium chloride and removing the solvent terahydrofuran by distillation.After being recrystallized in ethyl acetate and decoloured with active carbon,refined ethanesulphonamide was obtained with w(EtSO 2NH 2)≥99% and total yield≥85%(based on ethyl mercaptan).