HRID1693366

反应详情

EQUATION

反应方程式

HRID 1693366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydroxide solution (1.1 mL, 2M, 2.23 mmol) was added to a solution of 5-bromo-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid ethyl ester (Preparation 26, 500 mg, 1.86 mmol) in ethanol (20 mL), and the reaction mixture heated under reflux for 1.5 h and then concentrated in vacuo. The residue was dissolved in water (15 mL) and acidified with acetic acid resulting in formation of a brown precipitate. The solid was collected by filtration and dried to give the title compound as a brown solid. δH (d6 DMSO): 7.08 (1H, s), 7.97 (1H, s), 8.60 (1H, s); m/z (ES+)=241 [M+H]+.

WORKUP

后处理

  1. temperaturethe reaction mixture heated
  2. temperatureunder reflux for 1.5 h
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in water (15 mL)
  5. filtrationThe solid was collected by filtration
  6. customdried