反应详情

In 100 ml of toluene, 5 g (25.91 mmol) of 3,4-difluorobromobenzene, 13.39 g (155.45 mmol) of piperazine, 3.49 g (36.27 mmol) of sodium tert-butoxide, 0.24 g (0.26 mmol) of tris(dibenzylidene-acetone)dipalladium and 0.48 g (0.78 mmol) of BINAP are stirred under reflux overnight. Ethyl acetate is added, the mixture is then washed with water and the organic phase is extracted with 1N hydrochloric acid. The aqueous phase is then washed with ethyl acetate and subsequently adjusted to pH 8. Using dichloromethane, the product is extracted from the aqueous phase. The extract is then dried over magnesium sulphate, the solvent is removed and the target compound is dried under reduced pressure.

1. temperatureunder reflux overnight
2. washthe mixture is then washed with water
3. extractionthe organic phase is extracted with 1N hydrochloric acid
4. washThe aqueous phase is then washed with ethyl acetate
5. extractionUsing dichloromethane, the product is extracted from the aqueous phase
6. dry with materialThe extract is then dried over magnesium sulphate
7. customthe solvent is removed
8. customthe target compound is dried under reduced pressure