HRID1013748

反应详情

EQUATION

反应方程式

HRID 1013748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A pressure bottle was charged with (S)-7,7-difluoro-hexahydropyrrolo[1,2-a]pyrazine-1,4-dione (350 mg, 1841 μmol) and THF under nitrogen, and the solution was cooled to 0° C. under nitrogen. Lithium aluminum hydride (3681 μl, 3681 μmol) was added, the mixture was allowed to warm to RT, followed by heating at reflux for 3 h. 2 mL of water was carefully added, followed by 2 mL of 6N NaOH. After stirring for 10 min, the mixture was filtered through Celite and washed with EtOAc. The filtrate was concentrated. GC/MS: [M+H]=163.

WORKUP

后处理

  1. temperatureto warm to RT
  2. temperatureby heating
  3. temperatureat reflux for 3 h
  4. filtrationthe mixture was filtered through Celite
  5. washwashed with EtOAc
  6. concentrationThe filtrate was concentrated