反应详情

A solution of 1.0 g (5.15 mmoles) of 2,4-dihydroxy-3-propylacetophenone, see R. A. Appleton et al. in J. Med. Chem. 1977, 20, pages 371-379, and 1.77 g (7.7 mmoles) of methyl 4-bromomethylbenzoate in 20 ml of acetone was treated with 784 mg (5.66 mmoles) of K2CO3 and stirred at reflux for 15 hours. The reaction mixture was diluted with ether, washed with water and saturated aqueous NaHCO3 solution and dried with MgSO4. Evaporation of the solvent gave an oil which crystallized. This material was purified by chromatography on silica gel with 30% hexane/dichloromethane as eluent to provide 1.212 g (69% yield) of the title compound as a white powder mp 99.5°-100.5° C.

1. temperatureat reflux for 15 hours
2. washwashed with water and saturated aqueous NaHCO3 solution
3. dry with materialdried with MgSO4
4. customEvaporation of the solvent
5. customgave an oil which
6. customcrystallized
7. customThis material was purified by chromatography on silica gel with 30% hexane/dichloromethane as eluent