HRID512580

反应详情

EQUATION

反应方程式

HRID 512580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

4-(2-Ethyl-4-hydroxyphenyl)-2,2,6,6-tetramethylpyran-3,5-dione (0.100 g, 0.34 mmol) is added to a mixture of 2-fluoro-5-trifluoromethylpyridine (0.061 g, 0.41 mmol) and potassium carbonate (0.110 g, 0.69 mmol) in N,N-dimethylformamide (2 ml), and the mixture is heated at 140° C. under microwave irradiation for 1 hour. The mixture is cooled to room temperature, then acidified by addition of 2M aqueous hydrochloric acid. The mixture is diluted with dichloromethane and passed through a phase separation cartridge. The organic phase is concentrated to around 2 ml, and purified by preparative reverse phase HPLC to give 4-[4-(5-trifluoromethylpyridin-2-yloxy)-2-ethylphenyl]-2,2,6,6-tetramethylpyran-3,5-dione.

WORKUP

后处理

  1. temperatureThe mixture is cooled to room temperature
  2. custompassed through a phase separation cartridge
  3. concentrationThe organic phase is concentrated to around 2 ml
  4. custompurified by preparative reverse phase HPLC