HRID648249
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To the m-phenoxybenzyl ester of N-(p-trifluoromethylphenyl)valine (1.57 g) in about 15 ml benzene, with stirring and under nitrogen, is added N-chlorosuccinimide (0.53 g). The reaction mixture is heated to reflux for about 2 hours. The reaction is cooled and partitioned between ether and water. Aqueous phase is back-extracted with ether. The combined ether phases are washed with water and brine, dried over sodium sulfate, filtered and evaporated. The reaction product is put on preparative TLC plates and eluted using 10% ether/hexane to yield the m-phenoxybenzyl ester of N-(2-chloro-4-trifluoromethylphenyl)valine, MS m/e 477.1 (M+).
WORKUP
后处理
- temperatureThe reaction mixture is heated
- temperatureto reflux for about 2 hours
- temperatureThe reaction is cooled
- custompartitioned between ether and water
- extractionAqueous phase is back-extracted with ether
- washThe combined ether phases are washed with water and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- washeluted