HRID1295870

反应详情

EQUATION

反应方程式

HRID 1295870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

To a cooled (−5° C.) and stirred solution of LAH (1 M, 7.6 ml) in dry THF (75 ml) was added a solution of (1-benzyl-pyrrolidin-3-ylmethyl)-carbamic acid tert-butyl ester (1.47 g, 5.06 mmol) in THF (22 ml) over 20 minutes. The mixture was then heated at reflux for 2.5 hrs and cooled to room temperature and quenched by successive addition of ethyl acetate (50 ml). The organic layer was then washed with water (2×), 10% NaOH and brine, dried and evaporated to give the desired product in 90% yield.

WORKUP

后处理

  1. temperatureThe mixture was then heated
  2. temperatureat reflux for 2.5 hrs
  3. temperaturecooled to room temperature
  4. customquenched by successive addition of ethyl acetate (50 ml)
  5. washThe organic layer was then washed with water (2×), 10% NaOH and brine
  6. customdried
  7. customevaporated