HRID889037

反应详情

EQUATION

反应方程式

HRID 889037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidine-3-carboxylic acid (0.35 g, 1.28 mmol) in diethyl ether (5 ml) was added to a solution of lithium aluminium hydride (0.097 g, 2.56 mmol) in THF (5 ml) at temperature 0° C. over a period of 10 min. The mixture was refluxed for 2 hours and then stirred at room temperature for 20 hours. The reaction mixture was diluted with diethyl ether (15 ml) and quenched with water (10 ml). The organic layer was separated and aqueous layer was extracted with diethyl ether. The combined organic layer was washed with saturated brine solution, dried over Na2SO4 and evaporated to obtain a residue which was purified by preparative TLC to afford [1-(3-trifluoromethyl-phenyl)-pyrrolidin-3-yl]-methanol as a colorless mass (0.2 g, 64%).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 hours
  2. customquenched with water (10 ml)
  3. customThe organic layer was separated
  4. extractionaqueous layer was extracted with diethyl ether
  5. washThe combined organic layer was washed with saturated brine solution
  6. dry with materialdried over Na2SO4
  7. customevaporated
  8. customto obtain a residue which
  9. customwas purified by preparative TLC