摘要
用苯丙酸乙酯与草酸二乙酯合成α 羰基苯丁酸。采用一锅法代替文献中的两步反应 ,用稀硫酸代替文献中盐酸 -醋酸混酸水解 ,并用正交设计法对工艺条件进行优化 ,得出最佳工艺条件为 :n(苯丙酸乙酯 )∶n (草酸二乙酯 ) =1 0∶4 0 ,缩合 1 5h ,用w (H2 SO4) =2 0 %的硫酸水解15h ,产品收率由文献值的 5 7 2 %提高到 89%
Synthesis of 2 oxo 4 phenylbutyric acid was conducted in one pot.Ethyl 3 phenylpropionate condensed with diethyl oxalate in the presence of sodium methoxide,then the reaction mixture was hydrolyzed with dilute sulfuric acid directly.The optimum reaction conditions were: m (ethyl 3 phenylpropionate)∶ m (diethyl oxalate)=1∶4,time of condesation 1 5 h and hydrolysis for 15 h with sulfuric acid 〔w(H 2SO 4)=20%〕. The yield reached as high as 89% as compared with 57 2% in the literature.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2002年第5期289-290,294,共3页
Fine Chemicals
基金
浙江省自然科学基金资助项目 (2 0 0 0 16)
关键词
α-羰基苯丁酸
苯丙酸乙酯
草酸二乙酯
oxo 4 phenylbutyric acid
ethyl 3 phenylpropionate
diethyl oxalate