HRID1295870
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was then heated
- temperatureat reflux for 2.5 hrs
- temperaturecooled to room temperature
- customquenched by successive addition of ethyl acetate (50 ml)
- washThe organic layer was then washed with water (2×), 10% NaOH and brine
- customdried
- customevaporated