对羟基苯乙酸-N,N-二甲基甲酰氨基甲酰甲酯的合成工艺研究

Study on synthesis process of p-hydroxyphenyl acetic acid-N,N-dimethylformamide,dimethyl carbamyl

采用N,N-二甲基-2-氯乙酰胺、4-羟基苯乙酸、三乙胺等为原料,于乙腈中反应,HPLC跟踪检测合成对羟基苯乙酸-N,N-二甲基甲酰氨基甲酰甲酯(简称化合物B)。结果表明,最佳合成工艺参数为:反应时间12 h,反应温度60℃,溶剂用量为2 200 m L,物料比为n(4-羟基苯乙酸)∶n(N,N-二甲基-2-氯乙酰胺)=1∶1.10。在最佳条件下,收率86%,纯度98%以上。

Using N,N-dimethyl-2-chloro-acetamide,4-hydroxyphenyl acetic acid,triethylamine,etc. as raw materials,the reaction in acetonitrile,HPLC trace detection hydroxyphenyl acetic acid synthesis-N,N-dim-ethylformamide,carbamoyl ester（ compound B）. The result showed that the optimal synthesis parameters：reaction time 12 h,the reaction temperature is 60 ℃,the amount of solvent is 2 200 mL,material ratio of N（4-hydroxyphenyl acetic acid）：N（N,N-dimethyl-2-chloroacetamide）= 1：1. 10. Under optimal con-ditions the yield was 86%,with a purity of over 98%.