Hao Li-yong
2002
Citations
0
Influential Citations
0
Citations
Journal
Fine chemicals
Abstract
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).