反应详情

1 g (5.71 mmol) of 3-fluorobromobenzene and 2.95 g (34.29 mmol) of piperazine are dissolved in 20 ml of toluene, and 0.77 g (8 mmol) of sodium tert-butoxide is added. In the presence of 0.11 g (0.17 mmol) of BINAP and 0.05 g (0.06 mmol) of tris(dibenzylideneacetone)dipalladium, the mixture is then stirred under reflux overnight. After cooling, ethyl acetate is added and the mixture is washed with water. The mixture is then extracted with 1N hydrochloric acid, and the aqueous phase is washed with ethyl acetate. The pH is adjusted to 8–9 and the mixture is then extracted with dichloromethane. The organic phase is dried over magnesium sulphate and the solvent is removed, giving the target compound.

1. temperatureunder reflux overnight
2. temperatureAfter cooling
3. washthe mixture is washed with water
4. extractionThe mixture is then extracted with 1N hydrochloric acid
5. washthe aqueous phase is washed with ethyl acetate
6. extractionthe mixture is then extracted with dichloromethane
7. dry with materialThe organic phase is dried over magnesium sulphate
8. customthe solvent is removed
9. customgiving the target compound