HRID889033

反应详情

EQUATION

反应方程式

HRID 889033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
12.5 °C

PROCEDURE

实验过程

A mixture of 2-oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidine-3-carboxylic acid ethyl ester obtained in step 2 (0.5 g, 1.6 mmol) and ethanol were cooled to 10-15° C. Sodium borohydride (0.126 g, 3.3 mmol) was added portion wise over a period of 20 min and the reaction mixture was stirred for 3.5 hrs at 20-25° C. The organic volatiles were evaporated and the residue was taken into brine solution (15 ml). The aqueous layer was extracted with ethyl acetate, dried over Na2SO4 and evaporated to obtain brown semi solid which was purified by preparative TLC to afford 3-Hydroxymethyl-1-(3-trifluoromethyl-phenyl)-pyrrolidin-2-one as a colorless oil (0.177 g, 43%).

WORKUP

后处理

  1. customThe organic volatiles were evaporated
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. dry with materialdried over Na2SO4
  4. customevaporated
  5. customto obtain brown semi solid which
  6. customwas purified by preparative TLC