2-羟基-2-苯基乙酸异丙酯的合成

Synthesis of Isopropyl 2-hydroxy-2-phenylacetate

以1-羟基苯乙酸为原料,以二氯甲烷为溶剂,搅拌降温至0℃以下滴加二氯亚砜,(0±5)℃保温反应2 h,升温至室温反应4 h。TLC监控反应完,减压浓缩干得到2-羟基-2-苯基乙酰氯,浓缩物中加入异丙醇升温回流2 h,TLC监控反应完,减压浓缩至干,用二氯甲烷溶解,经中和、洗涤、干燥、浓缩、乙酸乙酯重结晶等步骤得到2-羟基-2-苯基乙酸异丙酯。综合收率为64.26%。该反应条件易于控制,操作简单,原料转化率高。

Using 1-hydroxyphenylacetic acid as raw material,and dichloromethane as solvent,the reaction was stirred and cooled to below 0℃,thionyl chloride was added dropwise,maitaining at(0±5)℃for 2 h,heated to room temperature and maitaining for 4 h.TLC monitoring the reaction,the mixture was concentrated to dryness to give 2-hydroxy-2-phenylacetyl chloride.The mixture was added with isopropyl alcohol and refluxed for 2 h.The reaction was monitored by TLC,concentrated to dryness under reduced pressure,dissolved in dichloromethane,neutralized,washed and dried,then concentrated,recrystallized in ethyl acetate to give 2-hydroxy-2-phenylacetic acid isopropyl ester.The overall yield was 64.26%.The reaction conditions were easy to control,the operation was simple,and the conversion rate of raw materials was high.