反应详情

温度

70 °C

A mixture of 6-benzyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4(3H)-one (5.0 g, 0.02 mol), phosphoryl chloride (3.30 mL, 0.035 mol) and acetonitrile (80 mL) and DMF (catalytic amount) was heated at 70° C. for 1 hour. The mixture was concentrated in vacuo and the remaining black residue was taken up in dichloromethane (250 mL) and poured over ice. The mixture was carefully neutralized with the addition of solid sodium bicarbonate. The organic layer was separated and dried over sodium sulfate and concentrated in vacuo. The mixture was purified by silica gel column with EtOAc/hexane (0-100%) to yield the title compound as a yellow oil (3 g, 57.8%).

1. concentrationThe mixture was concentrated in vacuo
2. additionpoured over ice
3. additionThe mixture was carefully neutralized with the addition of solid sodium bicarbonate
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe mixture was purified by silica gel column with EtOAc/hexane (0-100%)