反应详情

To an ethyl acetate (100 mL) solution of tert-butyl 3-(2-chloro-6-fluoro-4-trifluoromethylphenyloxy)-5-methylpyrazole-1-carboxylate (49.7 g, 126 mmol) was added 3 mol/L of HCL (40 mL), and the mixture was refluxed under heating for 2 hours. After completion of the reaction, the reaction mixture was consecutively washed with water and a 1 mol/L sodium hydroxide aqueous solution and dried over anhydrous magnesium sulfate, and the solvent was distilled off to give a white solid of 3-(2-chloro-6-fluoro-4-trifluoromethylphenyloxy)-5-methylpyrazole (33.0 g, yield: 89.0%). Melting point: 116˜117° C., 1H-NMR (CDCl3, TMS, ppm): δ2.24 (s, 3H), 5.69 (s, 1H), 7.36 (dd, J=1.8 Hz, JHF=9.4 Hz, 1H), 7.50-7.60 (m, 1H), 9.00-9.30 (brs, 1H).

1. temperaturethe mixture was refluxed
2. temperatureunder heating for 2 hours
3. customAfter completion of the reaction
4. washthe reaction mixture was consecutively washed with water
5. dry with materiala 1 mol/L sodium hydroxide aqueous solution and dried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off