HRID355950

反应详情

EQUATION

反应方程式

HRID 355950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.2 gm of lithium aluminum hydride was suspended in 110 ml of dried THF and stirred for 1 hour at room temperature. To the suspension was slowly added over 15 minutes a solution of 5 gm of the compound prepared in (2) above in 50 ml of THF. The mixture was stirred for 12 hours at room temperature, and after the addition of 20 ml of ethyl acetate, for a further 3 hours. Then, 5 ml of saturated aqueous solution of ammonium chloride was added to the mixture, followed by further stirring for 30 minutes. After removing the precipitate by filtration, the filtrate was washed with water and then with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated to obtain 4.27 gm of the title compound.

WORKUP

后处理

  1. stirringThe mixture was stirred for 12 hours at room temperature
  2. waitfor a further 3 hours
  3. stirringby further stirring for 30 minutes
  4. customAfter removing the precipitate
  5. filtrationby filtration
  6. washthe filtrate was washed with water
  7. dry with materialwith saturated brine, and dried over anhydrous sodium sulfate
  8. customThe solvent was evaporated