HRID550897

反应详情

EQUATION

反应方程式

HRID 550897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 260 mg of methyl 3-(4-aminophenyl)-1H-pyrrolo[2,3-b]pyridine-2-carboxylate in 30 mL of a 7N solution of ammonia in methanol are added 5 mL of 22% aqueous ammonia solution. The reaction mixture is then stirred for 20 hours in an autoclave at 80° C. (12.6 bar) and then concentrated under reduced pressure. The residue obtained is chromatographed on a column of silica (eluent: 9/1 dichloromethane/methanol by volume). The fractions containing the expected product are concentrated under reduced pressure. 140 mg of 3-(4-aminophenyl)-1H-pyrrolo[2,3-b]pyridine-2-carboxamide are obtained in the form of a pale yellow solid, the characteristics of which are as follows:

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customThe residue obtained
  3. customis chromatographed on a column of silica (eluent: 9/1 dichloromethane/methanol by volume)
  4. additionThe fractions containing the expected product
  5. concentrationare concentrated under reduced pressure