反应详情

To a stirred suspension of 3-hydroxyphthalic acid dimethyl ester (1.1 g, 5.2 mmol) in acetone (45 mL) and potassium carbonate (2.2 g, 15.7 mmol) was added 1-bromomethyl-3-methoxy-benzene (0.77 mL, 5.5 mmol) and refluxed for three hours. The solvent was evaporated and the residue was partitioned between water (50 mL) and ethyl acetate (80 mL) and washed with water (2×50 mL). The combined organic phases was dried, concentrated and purified by flash column chromatography (EtOAc/Hexane) to give 3-(3-methoxy-benzyloxy)-phthalic acid dimethyl ester (2.1 g, 118% crude yield). The product was used in the next step without further purification.

1. temperaturerefluxed for three hours
2. customThe solvent was evaporated
3. customthe residue was partitioned between water (50 mL) and ethyl acetate (80 mL)
4. washwashed with water (2×50 mL)
5. customThe combined organic phases was dried
6. concentrationconcentrated
7. custompurified by flash column chromatography (EtOAc/Hexane)