反应详情

tert-Butylamine (5.28 g, 72 mmol) was added to 5-bromo-2,4-dichloropyrimidine (15 g, 66 mmol) and triethylamine (19.9 g, 197 mmol) in acetonitrile (450 mL) at room temperature and the mixture was stirred at room temperature for 16 hours. Then the mixture was evaporated in vacuo and the crude residue was partitioned between EtOAc (450 mL) and water (400 mL). The organic layer was separated, washed with brine (400 mL) then dried over sodium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (hexane:EtOAc 88:12) to afford the title compound as a yellow oil in 52% yield, 8.8 g.

1. customThen the mixture was evaporated in vacuo
2. customthe crude residue was partitioned between EtOAc (450 mL) and water (400 mL)
3. customThe organic layer was separated
4. washwashed with brine (400 mL)
5. dry with materialthen dried over sodium sulfate
6. customevaporated in vacuo
7. customThe residue was purified by column chromatography on silica gel (hexane:EtOAc 88:12)