HRID388515

反应详情

EQUATION

反应方程式

HRID 388515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After dissolving 4-amino-2,5-difluorophenol (4.95 g) in dimethyl sulfoxide (50 ml) under a nitrogen stream, potassium tert-butoxide (4.05 g) was added at room temperature and the mixture was stirred for 25 minutes. After adding 4-chloropyridine-2-carboxyamide (2.70 g) to the mixture, stirring was continued at 80° C. for 2.5 hours. After cooling the reaction mixture to room temperature, a 1N aqueous solution of sodium hydroxide (74.25 ml) was added and stirring was continued for 10 hours. The precipitated solid was collected by filtration and washed with water. The solid was dried with warm air at 100° C. for 24 hours to give the title compound (3.38 g, 74%) as purple powder.

WORKUP

后处理

  1. additionwas added at room temperature
  2. stirringstirring
  3. waitwas continued at 80° C. for 2.5 hours
  4. stirringstirring
  5. waitwas continued for 10 hours
  6. filtrationThe precipitated solid was collected by filtration
  7. washwashed with water
  8. customThe solid was dried
  9. temperaturewith warm air at 100° C. for 24 hours