反应详情

温度

75 °C

36.2 g (358 mmol) of triethylamine and 54.3 g (358 mmol) of diethylthiocarbamoyl chloride are added in succession to a suspension of 36.7 g (325 mmol) of 2-fluoro-3-hydroxypyridine in 150 ml of toluene at room temperature, and the reaction mixture is heated at 75° C. After the reaction mixture has been stirred at this temperature for 1 hour, it is cooled to room temperature, diluted with ethyl acetate, washed 3 times with water, dried over Na2SO4 and concentrated in vacuo at 60° C.; 80 g of brown oil which, after recrystallization from Et2O/hexane, gave 64.2 g (86%) of brown crystals of m.p. 52°-54° C.

1. temperatureit is cooled to room temperature
2. washwashed 3 times with water
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo at 60° C.
5. custom80 g of brown oil which, after recrystallization from Et2O/hexane