反应详情

A solution of 1-(2-hydroxy-4-methoxyphenyl)propan-1-one (1 g, 5.55 mmol) in DMF (50 ml) is treated with potassium carbonate (0.920 g, 6.66 mmol) and stirred at RT for approximately 10 mins. 1-Bromo-2-methoxyethane (0.771 g, 5.55 mmol) is added and the mixture is stirred at RT overnight. The solvent is removed in vacuo and the residue is partitioned between in EtOAc/H2O. The organic phase is separated and washed with sat Na2CO3, 1M HCl, brine, dried (MgSO4) and concentrated in vacuo to afford a dark green/brown oil. Purification by chromatography on silica gel (50 g+70 g) eluting with 20% EtOAc/iso-hexane affords the title compound; MS m/z 239.2 [M+H]+.

1. stirringthe mixture is stirred at RT overnight
2. customThe solvent is removed in vacuo
3. customthe residue is partitioned between in EtOAc/H2O
4. customThe organic phase is separated
5. washwashed with sat Na2CO3, 1M HCl, brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo
8. customto afford a dark green/brown oil
9. customPurification by chromatography on silica gel (50 g+70 g)
10. washeluting with 20% EtOAc/iso-hexane