HRID478929

反应详情

EQUATION

反应方程式

HRID 478929 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-(R)-Prolylpyrrolidine (1.2 g, 7.1 mmol) was dissolved in THF (10 ml). The reaction mixture was cooled to 0° C. and BH3, 1M in THF (10 ml, 10 mmol) was dropwise at 0 C. The reaction mixture was refluxed for 16 h, 3 M HCl (4.7 ml). 2 M NaOH solution was added until pH 10 was reached. The product was extracted with 5% MeOH in CH2Cl2 (three times). The organic layers were dried over Na2SO4 and the solvent was removed to provide the title compound as a slightly yellow liquid (73%), which was used without further purification for the next step.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 16 h
  2. extractionThe product was extracted with 5% MeOH in CH2Cl2 (three times)
  3. dry with materialThe organic layers were dried over Na2SO4
  4. customthe solvent was removed