反应详情

Br2 (2.62 mL, 52 mmol) was added to 2-benzyl-3-methyl-3H-pyrimidin-4-one (Step 2, 9.3 g, 47 mmol) in CHCl3 (100 mL) and sat NaHCO3 (100 mL). After 30 min, the organic layer was separated, dried (Na2SO4) and filtered through a plug of silica. The filtrate was concentrated under reduced pressure, and azeotroped with CHCl3 (2×). The crude compound was dried under high vacuum for 16 h to provide the title compound. MS (ESI pos. ion) m/z: 279.0, 281.1. Calc'd for C12H11BrN2O: 278.01.

1. customthe organic layer was separated
2. dry with materialdried (Na2SO4)
3. filtrationfiltered through a plug of silica
4. concentrationThe filtrate was concentrated under reduced pressure
5. customazeotroped with CHCl3 (2×)
6. dry with materialThe crude compound was dried under high vacuum for 16 h