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
To an ethanol (10 mL) solution of methyl 3-(2-chloro-6-fluoro-4-trifluoromethylphenyloxy)-5-methylpyrazole-1-carboxylate (0.53 g, 1.5 mmol) was added 5% sodium hydroxide (8 mL), and the mixture was refluxed under heating for 2 hours. After completion of the reaction, the solvent was distilled off the reaction mixture, and then water was added, followed by extraction with ethyl acetate. The organic layers combined were washed with water, and dried over anhydrous magnesium sulfate and the solvent was distilled off. The resultant residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5) to give a white solid of 3-(2-chloro-6-fluoro-4-trifluoromethylphenyloxy)-5-methylpyrazole (0.39 g, yield: 88.2%).
WORKUP
后处理
- temperaturethe mixture was refluxed
- temperatureunder heating for 2 hours
- customAfter completion of the reaction
- distillationthe solvent was distilled off the reaction mixture
- additionwater was added
- extractionfollowed by extraction with ethyl acetate
- washThe organic layers combined were washed with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off
- customThe resultant residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5)