HRID751610

反应详情

EQUATION

反应方程式

HRID 751610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid ethyl ester (Preparation 14, 310 mg, 1.6 mmol) in ethanol (20 mL) was added 2N sodium hydroxide solution (1 mL, 2.0 mmol) and the reaction mixture heated under reflux for 1.5 h then concentrated in vacuo. The residue was dissolved in water (10 mL) and acidified with acetic acid giving an immediate brown precipitate. The solid was filtered and dried to give the title compound as a beige solid. δH (D2O): 7.11 (1H, s), 7.99 (1H, d), 8.05 (1H, d), 8.85 (1H, s); m/z (ES+)=163 [M+H]+.

WORKUP

后处理

  1. temperaturethe reaction mixture heated
  2. temperatureunder reflux for 1.5 h
  3. concentrationthen concentrated in vacuo
  4. dissolutionThe residue was dissolved in water (10 mL)
  5. filtrationThe solid was filtered
  6. customdried