反应详情

Benzyl bromide (30 mL) was added to a mixture of 1-(5-chloro-2,4-dihydroxy-phenyl)-ethanone (20 g, 0.107 moles) and potassium carbonate (37 g, 2.5 equiv) in acetonitrile (350 mL). The mixture was heated at reflux for 6 hours then allowed to cool and stirred overnight. The mixture was filtered and the solids were washed with dichloromethane (3×100 mL). The combined organic extracts were evaporated in vacuo to leave a pale yellow solid which was triturated with a mixture of hexane (350 mL)/ethyl acetate (15 mL) and filtered to give an off-white solid, 1-(2,4-bis-benzyloxy-5-chloro-phenyl)-ethanone (35.4 g, 90%). 1H NMR (400 MHz) consistent with structure.

1. temperatureThe mixture was heated
2. temperatureat reflux for 6 hours
3. temperatureto cool
4. filtrationThe mixture was filtered
5. washthe solids were washed with dichloromethane (3×100 mL)
6. customThe combined organic extracts were evaporated in vacuo
7. customto leave a pale yellow solid which
8. customwas triturated with a mixture of hexane (350 mL)/ethyl acetate (15 mL)
9. filtrationfiltered