HRID1893707

反应详情

EQUATION

反应方程式

HRID 1893707 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

According to Scheme 1, Step 1: K2CO3 (11.5 mmol, 1.59 g) was added to a solution of ethyl 5-(trifluoromethyl)-1H-pyrazole-4-carboxylate (7.69 mmol, 1.60 g) in acetonitrile (24 mL) followed by 1-(chloromethyl)-4-methoxybenzene (8.46 mmol, 1.15 mL) and the reaction mixture was heated under reflux for 4.5 hours. After evaporation of the solvent, the reaction mixture was diluted with brine and EtOAc. The aqueous phase was extracted with EtOAc. The organic phase was dried over MgSO4, was filtered and was concentrated under reduced pressure to yield ethyl 1-(4-methoxybenzyl)-3-(trifluoromethyl)-1H-pyrazole-4-carboxylate (7.68 mmol, 2.52 g, 100%) as an oil.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 4.5 hours
  3. customAfter evaporation of the solvent
  4. additionthe reaction mixture was diluted with brine and EtOAc
  5. extractionThe aqueous phase was extracted with EtOAc
  6. dry with materialThe organic phase was dried over MgSO4
  7. filtrationwas filtered
  8. concentrationwas concentrated under reduced pressure