摘要
用双三氯甲基碳酸酯(BTC)与对氯苯腙乙酸反应制备了对氯苯腙乙酰氯,对催化剂、溶剂、反应温度、反应物配比等影响反应的因素进行了研究,并通过正交试验研究确定了相关的反应条件,以二氯甲烷为溶剂,当反应温度为-5℃,n(BTC)∶n(对氯苯腙乙酸)=0.9∶1,n(N-甲基吡咯烷酮)∶n(对氯苯腙乙酸)=0.6∶1时,获得反应收率为87%.该方法具有原料廉价,操作简便等优点.
p-chlorophenylhydrazonoacetyl chloride was prepared using p-chlorophenylhydrazono acetic acid and bis（trichloromethyl） carbonate as starting materials. Effect of catalyst, solvent, temperature and ratio of reactants on the reaction was investigated. By orthogonal experimental design, the optimum experiment conditions were obtained as follows： using methylene dichloride as solvent, the reaction temperature was --5 ℃, the molar ratio of BTC to p-chlorophenylhydrazonoacetic acid was 0.9 ： 1, the molar ratio of N-methylpyrrolidone to p-chlorophenylhydrazonoacetie acid was 0.6 ： 1, and giving the product in 87 % yield. The advantages of this approach are inexpensive raw materials and simple preparation procedure.
出处
《浙江工业大学学报》
CAS
北大核心
2010年第4期376-379,共4页
Journal of Zhejiang University of Technology
关键词
双三氯甲基碳酸酯
对氯苯腙乙酸
对氯苯腙乙酰氯
bis （trichloromethyl） carbonate
p-chlorophenylhydrazonoacetic acid
p-chlorophenylhydrazonoacetyl chloride
