HRID552678

反应详情

EQUATION

反应方程式

HRID 552678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1.98 mmol rac-3-Hydroxy-3-(4-trifluoromethyl-phenyl)-pyrrolidine-1-carboxylic acid ethyl ester in 15 ml dioxane., was added 8 ml of a 2.5N solution of KOH in butanol. The solution was stirred under reflux for 2 hours. The solvent was removed in vacuo and the residue was taken in water. The aqueous phase was extracted 3 times with dichloromethane. The combined organic phases were dried over Na2SO4, evaporated and dried. The compound was suspended in hexane/ether (˜2:1), filtered and rinsed with hexane to yield the title compound (57%) as a light brown solid MS (m/e): 232.1 ([M+1], 100%).

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. customThe solvent was removed in vacuo
  3. extractionThe aqueous phase was extracted 3 times with dichloromethane
  4. dry with materialThe combined organic phases were dried over Na2SO4
  5. customevaporated
  6. customdried
  7. filtrationfiltered
  8. washrinsed with hexane