反应详情

温度

70 °C

To a suspension of 5-(benzyloxy)-2-(chloromethyl)-4H-pyran-4-one (1 10 g, 0.44 mol) in saturated aqueous NH4Cl (1 L) was added Zn powder (58.5 g, 0.9 mol) at r.t. and the mixture was stirred at 70° C. for 2 h. The mixture was partitioned between water and EtOAc, the EtOAc phase was collected and water phase was extracted with EtOAc twice. The combined EtOAc layer was washed with brine, dried over a2S04, and concentrated. The residue was purified by silica gel chromatography to give 40 g (42%) of 5-(benzyloxy)-2-methyl-4H-pyran-4-one.

1. customThe mixture was partitioned between water and EtOAc
2. customthe EtOAc phase was collected
3. extractionwater phase was extracted with EtOAc twice
4. washThe combined EtOAc layer was washed with brine
5. customdried over a2S04
6. concentrationconcentrated
7. customThe residue was purified by silica gel chromatography