反应详情

温度

80 °C

A mixture of 1-bromo-5-fluoro-4-nitro-2-(trifluoromethyl)benzene (16.0 g, 0.0556 mol), imidazole (4.0 g, 0.0588 mol) and N,N-diisopropylethylamine (10.1 mL, 0.0582 mol) in acetonitrile (160 mL) is stirred under nitrogen for 1.5 hour at 80° C. After concentration of the reaction mixture, the residue is partitioned between water and ethyl acetate. The aqueous phase is extracted with ethyl acetate, the combined organic phases are washed in turn with a saturated solution of ammonium chloride, brine and dried over sodium sulfate. Concentration and purification by cake filtration over silica gel, eluting with a mixture of ethyl acetate and cyclohexane from 2/8 to 1/1 affords the title compound as a yellow solid (16.1 g, 86.2%)

1. customAfter concentration of the reaction mixture, the residue is partitioned between water and ethyl acetate
2. extractionThe aqueous phase is extracted with ethyl acetate
3. washthe combined organic phases are washed in turn with a saturated solution of ammonium chloride, brine
4. dry with materialdried over sodium sulfate
5. concentrationConcentration and purification
6. filtrationby cake filtration over silica gel
7. washeluting with a mixture of ethyl acetate and cyclohexane from 2/8 to 1/1