3,3-二氯-2-羟基-4-羰基-4-对甲苯基丁酸乙酯的合成及工艺研究  

Synthesis of Ethyl 3,3-Dichloro-2-Hydroxy-4-Oxo-4-( p-tolyl) Butanoate

作　　者：王月梅 徐泽刚[1,2] 王伦 毛明珍[1,2] 宁斌科 李秉擘[1,2] 杨翠凤 Wang Yuemei;Xu Zegang;Wang Lun;Mao Mingzhen;Ning Binke;Li Bingbo;Yang Cuifeng(State Key Laboratory of Fluorine ＆ Nitrogen Chemicals,Shangxi Xi＇ an 710065;Xi＇an Mordem Research Institute,Shangxi Xi＇an 710065)

机构地区：[1]氟氮化工资源高效开发与利用国家重点实验室,陕西西安710065 [2]西安近代化学研究所,陕西西安710065

出　　处：《化工时刊》2018年第5期20-22,共3页Chemical Industry Times

摘　　要：以甲苯为起始原料,经过两步合成出3,3-二氯-2-羟基-4-羰基-4-对甲苯基丁酸乙酯。首先,甲苯与二氯乙酰氯发生傅克酰基化反应制备出中间体ɑ,ɑ-二氯对甲基苯乙酮,其次,通过中间体1,1-二氯对甲基苯乙酮与乙醛酸乙酯反应制备生成3,3-二氯-2-羟基-4-羰基-4-对甲苯基丁酸乙酯;通过条件优化,最终两步总收率71.9%。采用核磁共振、红外光谱对产品进行了结构表征。Ethyl 3,3-dichloro-2-hydroxy-4-oxo-4-（ p-tolyl） butanoate was synthesized from toluene through two steps. Firstly,the intermediate α,α-dichloro-1-（ p-tolyl） ethanone was synthesized by toluene and2,2-dichloroacetyl chloride. Secondly,ethyl 3,3-dichloro-2-hydroxy-4-oxo-4-（ p-tolyl） butanoate was synthesized by α,α-dichloro-1-（ p-tolyl） ethanone and ethyl glyoxylate solution. Under optimm conditions,the yield of two steps was 71. 9%. The structure of the title compound was characterized by IR,1 H NMR,13C NMR.

关 键 词：α α-二氯-4'-甲基苯乙酮 乙醛酸乙酯 合成 优化实验条件 

分 类 号：TQ245[化学工程—有机化工]