'一锅法'合成对羟基硫代苯甲酰胺

摘要

本文采用"一锅法"合成对羟基硫代苯甲酰胺.以对羟基苯甲醛为原料,甲酸为溶剂,氢氧化钠为缚酸剂,与盐酸羟胺反应生成对氰基苯酚.反应完毕后产物不经分离,直接向反应液中加入硫代乙酰胺和浓盐酸继续反应得到对羟基硫代苯甲酰胺,总收率为94.5%(以对羟基苯甲醛计).通过改变盐酸羟胺和氢氧化钠的用量、硫代乙酰胺的用量、浓盐酸的用量以及反应温度,确定了目标化合物的优化制备工艺条件.%The target compound,p-hydroxythiobenzamide was synthsized via an one-pot reaction.As the starting material,p-hydroxy-benzalehyde was reacted with hydroxylamine hydrochloride in the presence of sodium hydroxide in formic acid to generate p-hydroxybenzonitrile.After the completion of the reaction,thioacetamide and concentrated hydrochloric acid were added to the reac-tion mixturedirectly without separation to give p-hydroxythiobenzamide.The overall yield of the process was 94.5%,which was cal-culated by p-hydroxybenzaldehyde.And the optimal reaction conditions were determined by changing the amount of hydroxylamine hydrochloride and sodium hydroxide,the amount of thioacetamide,the amount of concentrated hydrochloric acid as well as the reac-tion temperature.