HRID1746667

反应详情

EQUATION

反应方程式

HRID 1746667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of cyclopentanone (10 g, 0.12 mol) and isobutyl amine (29.5 ml, 0.297 mol) was heated at 70° C. for 3 h under nitrogen. After cooling to 0° C., absolute ethanol (50 ml) was added to the reaction mixture, followed by sodium borohydride (6.59 g, 0.178 mol) in portions. The reaction mixture stirred at RT for 12 h, the solvent was removed under vacuum. The residue was taken up in MTBE and washed with water and brine. The organic layer was dried over Na2SO4, evaporated to dryness and the crude was purified by chromatography using silica gel (60-120 mesh), dichloromethane\methanol as eluent to afford of the titled compound as a yellow liquid.

WORKUP

后处理

  1. temperatureAfter cooling to 0° C.
  2. customthe solvent was removed under vacuum
  3. washwashed with water and brine
  4. dry with materialThe organic layer was dried over Na2SO4
  5. customevaporated to dryness
  6. customthe crude was purified by chromatography