HRID389098

反应详情

EQUATION

反应方程式

HRID 389098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

N,N′-carbonyldiimidazole (600 mg) was added to a solution of 3,5-difluoropyridine-2-carboxylic acid (500 mg) in THF (10 ml), followed by stirring at 50° C. for one hour. The reaction solution was returned to room temperature, a 40% methylamine/methanol solution (1 ml) was added thereto, followed by stirring at room temperature for one hour. The reaction solution was concentrated and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 0:100 linear gradient) to obtain 3,5-difluoro-N-methylpyridine-2-carboxamide (293 mg) as a colorless solid.

WORKUP

后处理

  1. customwas returned to room temperature
  2. stirringby stirring at room temperature for one hour
  3. concentrationThe reaction solution was concentrated
  4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 0:100 linear gradient)