HRID876246

反应详情

EQUATION

反应方程式

HRID 876246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

At 50° C., 11.35 g (40.96 mmol) of N-(5-bromopyridin-3-yl)benzamide, 11.67 g (61.43 mmol) of [4-(trifluoromethyl)phenyl]boronic acid and 8.68 g (81.91 mmol) of sodium carbonate were dissolved in 68 ml of 1,2-dimethoxyethane, 21 ml of water and 151 ml of DMF. The mixture was flushed with argon, 237 mg (0.21 mmol) of tetrakis(triphenylphosphine)palladium(0) were added and the mixture was stirred at 85° C. for 12 h. The reaction mixture was concentrated slightly on a rotary evaporator, diluted with water and extracted with dichloromethane. The organic phase was concentrated under reduced pressure and the residue was purified by column chromatography (cyclohexane/ethyl acetate 1:1). Yield: 10.6 g (76% of theory)

WORKUP

后处理

  1. additionwere added
  2. concentrationThe reaction mixture was concentrated slightly on a rotary evaporator
  3. additiondiluted with water
  4. extractionextracted with dichloromethane
  5. concentrationThe organic phase was concentrated under reduced pressure
  6. customthe residue was purified by column chromatography (cyclohexane/ethyl acetate 1:1)