HRID628529

反应详情

EQUATION

反应方程式

HRID 628529 的结构方程式

PROCEDURE

实验过程

A mixture of 5-(4-methoxy-2,5-dimethyl-phenyl)-1-methyl-3-trifluoromethyl-1H-pyrazole (described in Reference preparation example 84) 3.2 g, 6N aqueous hydrochloric acid solution 5.3 ml and tetrahydrofuran 50 ml was stirred with heating under reflux for one hour. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium carbonate solution and saturated saline. The organic layer was dried over anhydrous magnesium sulfate, and was then concentrated under reduced pressure. The resulting residue was subjected to a silica gel column chromatography to give 3-(4-methoxy-2,5-dimethyl-phenyl)-1-methyl-5-trifluoromethyl-1H-pyrazole 3 g.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for one hour
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated aqueous sodium carbonate solution and saturated saline
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationwas then concentrated under reduced pressure