HRID498054

反应详情

EQUATION

反应方程式

HRID 498054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1-(2-pyridinyl)-1H-pyrazol-5-ylamine (6.94 g, 43.3 mmol), 2-chloro-4,5-difluorobenzoic acid (10.0 g, 51.9 mmol), copper acetate (II) (0.787 g, 4.33 mmol) and potassium carbonate (5.98 g, 43.3 mmol) in N,N-dimethylformamide (40 mL) was heated under reflux under an argon atmosphere for 3 hours. The solution was allowed to cool to room temperature, and poured into water. The solution was made weakly acidic by the addition of 6N hydrochloric acid, and the resulting crude crystals were collected by filtration. The crystals were washed with water and air dried to give the title compound (8.99 g, 55% yield).

WORKUP

后处理

  1. temperatureunder reflux under an argon atmosphere for 3 hours
  2. filtrationthe resulting crude crystals were collected by filtration
  3. washThe crystals were washed with water and air
  4. customdried