N-(4-氯苯基)-N′-(3,4-二氯苯基)脲合成新工艺研究

Study on a New Technology for Synthesis of TCC

本文研究了N - (4-氯苯基 ) -N′- (3,4 -二氯苯基 )脲 (TCC)的合成新工艺 .通过 3,4 -二氯苯胺和对氯苯基异氰酸酯的反应制备TCC ,首先在反应瓶中加入 3,4 -二氯苯胺和溶剂 ,加热回流以至溶剂的饱和蒸汽充满反应瓶 ,隔绝空气 ,然后滴加对氯苯基异氰酸酯的邻二氯苯 -二甲苯溶液 ,控制在溶剂回流状态 (温度为 15 0～ 15 0℃ )下反应 4 0min ,反应完毕 ,冷却到 0～ 5℃ ,过滤 ,用适量反应溶剂滤饼 ,干燥 ,得到白色针状晶体 ,收率为 95 % ,是一种合成TCC的新工艺 .

The new technology for synthesis of TCC [N-(4-chloropheny1)-N′-(3,4-dichlorophenyl) urea] and o-dichloro-4-nitrobenaene is studied.TCC is prepared by,3,4-dichloroaniline and p-chlorophenyl isocyanate.The solution of p-chloropheny1 isocyanate and o-dichlorobenzene-xylene is added dropwise to the reaction vessel containing 3,4-dichloroaniline and solvnet.The mixture is stirred well and held at reflux temperature (150～150 ℃).After the reaction was completed,the mixture is cooled to 0～5 ℃,filtered and washed by the solvent and dried,hence fine colorless needles are gained in 95% yield.This is a new technology for synthesis of TCC.