摘要
以三氯乙酸和三氯乙酸钠为原料,室温下在DMF中制备三氯甲基负离子,进攻苯丙醛的羰基碳制得中间体4-苯基-1,1,1-三氯-2-丁醇,然后在强碱条件下水解制得目标产物2-羟基-4-苯基丁酸.采用正交试验法对合成2-羟基-4-苯基丁酸的控制步骤水解反应的条件进行了综合优化,得到最佳水解条件为:n(4-苯基-1,1,1-三氯-2-丁醇)∶n(NaOH)=1∶20;V(DME)∶V(H2O)=1∶1;搅拌速度550 r/min;水解时间24 h;水解收率57%;两步总产率54%.产物结构经元素分析、红外光谱1、H-NMR确认.
Intermedia 4-phenyl-1,1,1-trichloro-2-butanol was prepared from hydrocinnamaldenyde and trichloromethide anion made by trichloroacetic acid and sodium trichloroacetate undergoing addition in dimethyl formamide（DMF） at room temperature, and then was hydrolyzed with strong alkali to form target 2-hydroxy-4-phenylbutyric acid. The key step of hydrolysis was optimized, with 4-phenyl-1,1,1-trichloro-2-hutanol and sodium hydroxide in molar ratio 1 ： 20, water and dimethoxyethane （DME） in volume ratio 1 ： 1, the velocity of stirring 550 r/min, and time of hydrolysis 24 h. Hydrolysis was 57% and total yield of two steps was 54%. The product was identified by elementary analysis, IR and 1^ H-NMR.
出处
《江南大学学报（自然科学版）》
CAS
2006年第5期594-596,601,共4页
Joural of Jiangnan University (Natural Science Edition)
基金
国家自然科学基金项目(20476038)
教育部新世纪优秀人才计划项目(2006)
