反应详情

温度

25 °C

11.2 g (100 mmol) of potassium tert.-butoxide are added under an N2 atmosphere at 25° C. to 25 ml (183 mmol) of 4-trifluoromethylbenzyl alcohol. 7.2 g (50 mmol) of 4-chloro-2-picoline-N-oxide are subsequently added dropwise, then 10 ml of tert.-butanol are added, and the mixture is stirred for 1 hour at 25° C. and for 30 minutes at 75°-80° C. Water is then added and the mixture is extracted three times using dichloromethane, the extracts are dried and concentrated, and the residue is chromatographed on silica gel using dichloromethane/methanol. The product is obtained from the corresponding fractions, m.p. 113°-115° C.

1. extractionthe mixture is extracted three times
2. customthe extracts are dried
3. concentrationconcentrated
4. customthe residue is chromatographed on silica gel
5. customThe product is obtained from the corresponding fractions, m.p. 113°-115° C.