HRID1893707
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reaction mixture was heated
- temperatureunder reflux for 4.5 hours
- customAfter evaporation of the solvent
- additionthe reaction mixture was diluted with brine and EtOAc
- extractionThe aqueous phase was extracted with EtOAc
- dry with materialThe organic phase was dried over MgSO4
- filtrationwas filtered
- concentrationwas concentrated under reduced pressure