反应详情

1 M aq. Na2CO3 (20 mL) and ethanol (10 mL) were added to a solution of 5-chloropyrimidine hydrochloride (3.03 g, 20.06 mmol, prepared as described in WO 9821188), 4-formylphenylboronic acid (3.90 g, 26.01 mmol) and [1,4-bis(diphenylphosphino)butane]palladium(II) dichloride (0.60 g, 0.99 mmol) in toluene (40 mL) and the mixture was heated to reflux for 18 h. The cooled reaction mixture was diluted with ethyl acetate, washed with sat. aq. NaHCO3 and brine, dried (MgSO4), and concentrated. Purification by chromatography (SiO2, 4:1 hexane/ethyl acetate) yielded 1.80 g (42%) of the title compound. MS 185 (M+H)+.

1. temperaturethe mixture was heated
2. temperatureto reflux for 18 h
3. customThe cooled reaction mixture
4. washwashed with sat. aq. NaHCO3 and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customPurification by chromatography (SiO2, 4:1 hexane/ethyl acetate)