反应详情

Benzyl bromide (1.32 ml, 11.1 mmol) was added to a stirred solution of diethyl 1-(ethyloxy)-4-hydroxy-2,3-naphthalenedicarboxylate (2.45 g, 7.38 mmol) and potassium carbonate (1.53 g, 11.1 mmol) in acetone (50 ml). The reaction mixture was refluxed for 1 hour under an atmosphere of argon. The resulting mixture was evaporated and the residue was partitioned between 2× ethylacetate and brine. The combined organics were washed with water and dried over magnesium sulphate. The clear oil was purified by chromatography on silica gel, eluting with ethyl acetate (0-40%) in hexane to give the title compound as clear oil (3.05 g, 7.23 mmol). LC/MS: Rt=3.77, [MH]+ 423

1. temperatureThe reaction mixture was refluxed for 1 hour under an atmosphere of argon
2. customThe resulting mixture was evaporated
3. customthe residue was partitioned between 2× ethylacetate and brine
4. washThe combined organics were washed with water
5. dry with materialdried over magnesium sulphate
6. customThe clear oil was purified by chromatography on silica gel
7. washeluting with ethyl acetate (0-40%) in hexane