HRID923815

反应详情

EQUATION

反应方程式

HRID 923815 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

To a mixture of N2-methyl-5-trifluoromethylpyridine-2,3-diamine (3.82 g) and THE (40 ml), 2-ethylsulfanylbenzoic acid chloride (4.42 g) was added, stirred at 50° C. for 2 hours, then stirred under reflux for 2 hours. After the mixture was allowed to cool to room temperature, sodium hydrogen carbonate (1.85 g) was added thereto, and stirred at 50° C. for 2 hours. After the mixture was allowed to cool to room temperature, water was poured thereinto, and then the precipitated solid was collected by the filtration. The resulting solid was washed with water and hexane, and dried to give 7.15 g of N-(2-methylamino-5-trifluoromethylpyridine-3-yl)-2-ethylsulfanyl-benzamide (Compound ((1B)-19).

WORKUP

后处理

  1. stirringstirred
  2. temperatureunder reflux for 2 hours
  3. temperatureto cool to room temperature
  4. stirringstirred at 50° C. for 2 hours
  5. temperatureto cool to room temperature
  6. filtrationthe precipitated solid was collected by the filtration
  7. washThe resulting solid was washed with water and hexane
  8. customdried