HRID459423

反应详情

EQUATION

反应方程式

HRID 459423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.86 g (22.66 mmol) of LiAlH4 was added to a solution of 3.60 g (7.63 mmol) of B3 in 20 ml of anhydrous THF and stirred at reflux for 2 hours. After cooling, Arberlite® IR-120(plus) was added and stirring was continued until hydrogen evolution had ended. The mixture was filtered through Celite® and the solvent was subsequently removed under reduced pressure. The crude product was purified by means of column chromatography (CH2Cl2/MeOH=12:1). Yield: 0.84 g (84% of theory).

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. temperatureAfter cooling
  3. additionArberlite® IR-120(plus) was added
  4. stirringstirring
  5. filtrationThe mixture was filtered through Celite®
  6. customthe solvent was subsequently removed under reduced pressure
  7. customThe crude product was purified by means of column chromatography (CH2Cl2/MeOH=12:1)