反应详情

With efficient stirring, 27.6 g of 1-(2,4-dichlorophenyl)-2-fluoro-2-(1H-1,2,4-triazolyl)ethanol (prepared in accordance with Example P1a) were added to a mixture of 250 ml of 2n NaOH solution, 250 ml of diethyl ether and 0.5 g of tetrabutylammonium bromide. 25 ml of 4-nitrofluorobenzene are added at 20° C. to this mixture, which is stirred for another 20 hours at room temperature. The separated ethereal phase is washed with water until neutral, dried over sodium sulfate, filtered and concentrated by evaporation. The crude oily product (35 g) is purified by chromatography through silica gel and melts after recrystallisation from diisopropyl ether/cyclohexanone at 98°-100° C.

1. washThe separated ethereal phase is washed with water until neutral,
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated by evaporation
5. customThe crude oily product (35 g) is purified by chromatography through silica gel and melts
6. customafter recrystallisation from diisopropyl ether/cyclohexanone at 98°-100° C.