HRID2228753

反应详情

EQUATION

反应方程式

HRID 2228753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium aluminium hydride [1.0 mol soln. in tetrahydrofuran] (11.52 ml, 11.52 mmol) was added to a solution of (2R)-1-isobutyl-2-pyrrolidinecarboxamide (1.3 g, 7.68 mmol) [see preparation 59] in tetrahydrofuran (5 ml) @0° C. The reaction mixture was stirred for 10 mins and then heated to reflux for 6 hrs. Water (0.5 ml) was added to the cooled mixture followed by sodium hydroxide (1.5 ml) and water (1.5 ml). Tetrahydrofuran (10 ml) was added and the mixture was stirred at room temperature for 1 hr. The aluminium salts were removed by filtration and washed well with diethyl ether. The filtrate was then evaporated under reduced pressure to afford the title compound as a white solid, 705 mg, (58%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 6 hrs
  3. stirringthe mixture was stirred at room temperature for 1 hr
  4. customThe aluminium salts were removed by filtration
  5. washwashed well with diethyl ether
  6. customThe filtrate was then evaporated under reduced pressure