HRID2186735

反应详情

EQUATION

反应方程式

HRID 2186735 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Methyl (6-acetoxy-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-1-yl)acetate (1080 mg) was dissolved in THF (15 ml) under an argon atmosphere, and the resultant solution was stirred at 0° C. Lithium aluminum hydride (355 mg) was added to the solution, and the mixture was stirred at 0° C. After disappearance of the raw materials was confirmed, the reaction solution was added to water (100 ml), and then extracted with ethyl acetate. The resultant organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and then concentrated. The resultant residue was purified by column chromatography (silica gel:hexane/ethyl acetate=2/1) to obtain the object compound (624 mg, yield 81%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe resultant organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe resultant residue was purified by column chromatography (silica gel:hexane/ethyl acetate=2/1)