4-硝基-N-[3-(2-羟乙基)砜基]苯基苯甲酰胺的合成

Synthesis of 4-Nitro-N-[3-(2-hydroxyethyl)sulfonyl]phenylbenzoylamide

以3-(2-羟乙基砜基)苯胺和对硝基苯甲酸为主要原料,经过酰氯化和缩合两步反应合成了活性染料中间体4-硝基-N-[3-(2-羟乙基)砜基]苯基苯甲酰胺。研究了催化剂、卤化剂等对酰氯化反应的影响,实验得到酰氯化反应的较佳条件:DMF作催化剂,二氯亚砜作卤化剂,酰氯化产物收率可达97%。同时还考察了缩合反应较佳条件:n(3-(2-羟乙基砜基)苯胺)∶n(对硝基苯甲酰氯)=1.2∶1,反应温度30℃,反应时间2 h。在此条件下,缩合反应产物收率达到90%。产物及中间体的结构经过了IR1、H NMR鉴定。

4-Nitro-N-[ 3-（2-hydroxyethyl） sulfonyl-] phenylbenzoylamide was synthesized using 3-（2-hydroxyethylsulfonyl）aniline and 4-nitrobenzoic acid as starting materials through acyl chlorination and condensation. The effects of catalyst, halogenating agent on acyl chlorination results were studied. The results showed that DMF and thionyl chloride were suitable catalyst and halogenating agent respectively, the yield of acyl chlorination was 97%. And the obtained optimum conditions of condensation were n（3-（2-hydroxyethylsulfonyl） aniline）： n（4-nitrobenzoic acid）=1.2 ：1, reaction tem- perature 30℃, reaction time 2 h. Under above conditions, the yield was 90%. The structures of product and intermediate were characterized bv IR and ^1H NMR