HRID398039

反应详情

EQUATION

反应方程式

HRID 398039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At ice-bath temperature, lithium aluminium hydride (1.6 g, 42.16 mmol) was added in portions to a stirring mixture of (S)-2-benzyl piperazine-3,6-dione (3.0 g, 14.70 mmol) and tetrahydrofuran (80 ml). After 30 min at ice-bath temperature, the mixture was refluxed for 4 h with stirring. The reaction was quenched by the portionwise addition of sodium sulfate decahydrate and some methanol until hydrogen evolution ceased. It was filtered and the solids were washed several times with dichloromethane. The combined filtrates were evaporated to leave a white solid. MS (m/z): 177.1 (M+H)+; C11H16N2 requir. 176.3.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 4 h
  2. customThe reaction was quenched by the portionwise addition of sodium sulfate decahydrate
  3. filtrationIt was filtered
  4. washthe solids were washed several times with dichloromethane
  5. customThe combined filtrates were evaporated
  6. customto leave a white solid