反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of N-{3-[(6-aminopyridin-3-yl)oxy]phenyl}-3-(trifluoromethyl)benzamide (2.00 g, 5.36 mmol) in pyridine (60 mL) was added 4-methylbenzenesulfonyl chloride (1.12 g, 5.89 mmol) under ice-cooling, and the mixture was stirred with heating at 80° C. for 2 days. After cooling the reaction mixture to room temperature, water (200 mL) was added, and the mixture was extracted with ethyl acetate (300 mL). The organic layer was washed with saturated brine (300 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (2.75 g, 99%) as a yellow oil. The obtained compound was used for the next reaction without further purification.
WORKUP
后处理
- temperaturecooling
- temperatureAfter cooling the reaction mixture to room temperature
- extractionthe mixture was extracted with ethyl acetate (300 mL)
- washThe organic layer was washed with saturated brine (300 mL)
- dry with materialdried over anhydrous sodium sulfate
- filtrationThe insoluble material was filtered off
- concentrationthe filtrate was concentrated under reduced pressure