HRID580261

反应详情

EQUATION

反应方程式

HRID 580261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2-fluoro-4-chloro-5-hydroxyphenyl)-3,4,5-trimethylpyrazole (25.5 g), allyl bromide (13.3 g), anhydrous potassium carbonate (14.5 g) and acetonitrile (150 ml) was heated under reflux, with stirring for 3 hours. After cooling, the reaction mixture was filtered through a filter to remove the inorganic salts therefrom and the filtrate was concentrated to a small volume under reduced pressure, affording the titled compound (28.7 g) as a pale brown crystalline solid. Recrystallization of this solid from cyclohexane yielded a white crystalline solid. m.p. 97°-99° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. filtrationthe reaction mixture was filtered through
  5. filtrationa filter
  6. customto remove the inorganic salts
  7. concentrationthe filtrate was concentrated to a small volume under reduced pressure