HRID243563

反应详情

EQUATION

反应方程式

HRID 243563 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

2-(4-(4-benzylpiperazin-1-yl)cyclohexyl)-N,N-dimethylacetamide (800 mg) is dissolved in THF (20 ml) and cooled to 0° C. 2 M LiAlH4 in THF (2.3 ml) is added. The reaction mixture is warmed to room temperature and stirred for 1 hour. The reaction is quenched by slow addition of satd. aqueous K2CO3 (50 ml), then a potassium sodium tartrate solution (20 ml) is added. The mixture is diluted with EtOAc and the layers are separated. The aqueous layer is extracted with EtOAc (2×). The combined organic layers are dried (Na2SO4), filtered, and the solvent is removed under reduced pressure to give 2-(4-(4-benzylpiperazin-1-yl)cyclohexyl)-N,N-dimethylethanamine (660 mg). m/z(+) 330 (M+H+).

WORKUP

后处理

  1. temperatureThe reaction mixture is warmed to room temperature
  2. customThe reaction is quenched by slow addition of satd
  3. additionaqueous K2CO3 (50 ml), then a potassium sodium tartrate solution (20 ml) is added
  4. additionThe mixture is diluted with EtOAc
  5. customthe layers are separated
  6. extractionThe aqueous layer is extracted with EtOAc (2×)
  7. dry with materialThe combined organic layers are dried (Na2SO4)
  8. filtrationfiltered
  9. customthe solvent is removed under reduced pressure