HRID1389345

反应详情

EQUATION

反应方程式

HRID 1389345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for about 2 hours
  3. temperatureThe reaction is cooled
  4. custompartitioned between ether and water
  5. extractionAqueous phase is back-extracted with ether
  6. washThe combined ether phases are washed with water and brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated
  10. washeluted