机构地区: 广东药学院药科学院药物合成研究所
出 处: 《化学试剂》 2008年第12期927-928,934,共3页
摘 要: 以(+)-邻氯苯甘氨酸为原料,在氯化亚砜-甲醇溶液中直接反应成功的合成了标题化合物。考察了滴加氯化亚砜时的温度、原料与氯化亚砜的物质的量比,滴加完氯化亚砜后的反应温度、反应时间等因素对酯化和成盐产率的影响,并对其进行了优化,确定了最佳反应条件:当滴加氯化亚砜的温度为-5~0℃,原料与氯化亚砜的物质的量比1:2,滴加完氯化亚砜后的反应温度为50℃,反应时间为6h时,总产率达到98%。用IR对产物的结构进行了表征。 Methyl ( + )-alpha-amino (2-chlorophenyl) acetate hydrochloride was synthesized by reacting ( + )-alpha-amino (2- chlorophenyl) acetic acid with the methanol solution of thionyl chloride. The effects of the temperature of dropping thionyl chloride, the molar ratio of reactants, the reaction temperature after completion of trickling thionyl chloride and the reaction time on the yield of methyl( + )-alpha-amino(2-chlorophenyl)acetate hydrochloride were investigated. The optimum reaction conditions were specified as follows: the temperature of dropping thionyl chloride was between - 5℃ and 0℃, the molar ratio between (+)-alpha-amino(2-chlorophenyl)acetic acid and thionyl chloride was 1 : 2, the temperature after completion of dropping thionyl chloride was 50 ℃, the reaction time was 6 h, and the total yield reached 98 % . The structure of the product was characterized by the FTIR spectrometry.