HRID249875

反应详情

EQUATION

反应方程式

HRID 249875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

LiAlH4 (1 M solution in THF, 11 mL, 11.0 mmol) was added drop wise to solution of (S)-1-benzyl-3-ethylpiperazine-2-one (0.8 g, 3.66 mmol) in THF (30 mL) at 0° C. The reaction mixture was stirred at 65° C. for 17 h, then cooled 0° C. and quenched sequentially with H2O (0.7 mL), 10% NaOH (1 mL) and H2O (1.5 mL). Diethylether (100 mL) was added to the reaction mixture, and stirring was continued for 1.5 h. The solid was filtered off, the filtrate was concentrated and dried in vacuum to afford (S)-1-benzyl-3-ethylpiperazine (0.67 g, 87%) as an oily solid. 1H NMR and MS consistent.

WORKUP

后处理

  1. temperaturecooled 0° C.
  2. customquenched sequentially with H2O (0.7 mL), 10% NaOH (1 mL) and H2O (1.5 mL)
  3. additionDiethylether (100 mL) was added to the reaction mixture
  4. stirringstirring
  5. waitwas continued for 1.5 h
  6. filtrationThe solid was filtered off
  7. concentrationthe filtrate was concentrated
  8. customdried in vacuum