HRID1271237

反应详情

EQUATION

反应方程式

HRID 1271237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.86 g of (±)-3-(N-benzyloxycarbonylpyrrolidin-2-yl)acrylic acid ethyl ester in 15 ml of dry dichloromethane1, 12.9 ml of diisobutylaluminum hydride (1M toluene solution) was added dropwise under an argon atmosphere at −70° C. or lower, followed by stirring for one hour. To the reaction solution, 60 ml of 1N hydrochloric acid was added dropwise, and then the mixture was heated to room temperature and extracted with diethyl ether. The extract was washed with water and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 0.75 g of the desired compound as a colorless oily substance.

WORKUP

后处理

  1. extractionextracted with diethyl ether
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography