HRID1366657

反应详情

EQUATION

反应方程式

HRID 1366657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(4aR,8aS)-Octahydro-2,3-quinoxalinedione (4.67 g, 27.8 mmol) was added portion wise to 1M LAH (111 mL, 111 mmol) in diethyl ether (30 mL). The reaction was allowed to heated to reflux and stirred at reflux for 4 h. After cooling to room temperature, the reaction was quenched by the sequential addition of H2O (4.2 mL), 15% NaOH (4.2 mL), and H2O (12.6 mL). The mixture was stirred for 0.5 h, and the solids were filtered off and washed with excess EtOAc. The combined filtrates were concentrated under reduced pressure to provide (4aR,8aS)-decahydroquinoxaline as a white solid (3.6 g, 92%). LCMS: (M+H)+: 141.1.

WORKUP

后处理

  1. temperatureto heated
  2. temperatureto reflux
  3. temperatureat reflux for 4 h
  4. customthe reaction was quenched by the sequential addition of H2O (4.2 mL), 15% NaOH (4.2 mL), and H2O (12.6 mL)
  5. stirringThe mixture was stirred for 0.5 h
  6. filtrationthe solids were filtered off
  7. washwashed with excess EtOAc
  8. concentrationThe combined filtrates were concentrated under reduced pressure