反应详情

A mixture of 5-fluoro-2,4-bis[(trimethylsilyl)oxy]pyrimidine (1 g, commercially available from Lancaster), 1-bromo-3-chloropropane (0.44 mL) and I2 (10 mg) in 1,2-dichloroethane (10 mL) was heated to reflux for 30 h. Then the reaction mixture was treated with water and the pH was brought to 7 using aqueous 6N NaOH solution, the mixture was extracted twice with DCM, the organic phase dried over Na2SO4 and the solvent evaporated under reduced pressure. The crude product was purified by flash chromatography on silica gel eluting with DCM/MeOH 95/5 to give 35 mg of the title compound.

1. temperatureto reflux for 30 h
2. extractionthe mixture was extracted twice with DCM
3. dry with materialthe organic phase dried over Na2SO4
4. customthe solvent evaporated under reduced pressure
5. customThe crude product was purified by flash chromatography on silica gel eluting with DCM/MeOH 95/5