HRID2169425

反应详情

EQUATION

反应方程式

HRID 2169425 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred suspension of 1-pyrrolo[2,3-b]pyridin-1-yl-cyclopentanecarbonitrile (393) (6.2 g, 29.35 mmol) in water (90 mL) was added LiOH.H2O (14 g, 334.56 mmol). The reaction mixture was refluxed for 24 h (TLC, 30% ethyl acetate in hexane, Rf=0.3). It was thereafter cooled to 0° C. and the aqueous part was acidified with HCl (6N) to pH 3 and extracted with ethyl acetate (3×50 mL). The organic phase was thereafter dried and concentrated to get 1-pyrrolo[2,3-b]pyridin-1-yl-cyclopentanecarboxylic acid (394) (5.8 g, 86%) as an off-white solid.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×50 mL)
  2. customThe organic phase was thereafter dried
  3. concentrationconcentrated