反应详情

A solution of 3-(3-methoxy-benzyloxy)-phthalic acid dimethyl ester (2.0 g crude, 5.5 mmol) in reagent alcohol (100 mL) and 3 N sodium hydroxide (35 mL) was refluxed for two hours. The solution was evaporated and the residue was dissolved in water (80 mL) and washed with methylene chloride (3×70 mL) then acidified to pH around 4. The resulting mixture was extracted with ethyl acetate (2×60 mL) and the combined organic layers was washed with water (2×70 mL), dried and concentrated to give 3-(3-methoxy-benzyloxy)-phthalic acid as an off-white solid (1.6 g, 98% crude yield). The product was used in the next step without further purification.

1. customThe solution was evaporated
2. dissolutionthe residue was dissolved in water (80 mL)
3. washwashed with methylene chloride (3×70 mL)
4. extractionThe resulting mixture was extracted with ethyl acetate (2×60 mL)
5. washthe combined organic layers was washed with water (2×70 mL)
6. customdried
7. concentrationconcentrated