反应详情

A mixture of 4-(4-fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester (7.8 g, 15.4 mmol) lithium hydroxide monohydrate (1.8 g, 46.2 mmol) in tetrahydrofuran (60 mL) and water (60 mL) was stirred at room temperature for 72 h. The mixture was then evaporated followed by acidification to pH 2 at 0° C. with concentrated HCl. The organic layer was then diluted with ethyl acetate, separared, washed with water and dried over sodium sulfate. Filtration and half evaporation gave a white suspension which was filtered off and washed with ether to afford the title compound (2.5 g, 56%) as a white solid.

1. customThe mixture was then evaporated
2. customfollowed by acidification to pH 2 at 0° C. with concentrated HCl
3. additionThe organic layer was then diluted with ethyl acetate
4. washwashed with water
5. dry with materialdried over sodium sulfate
6. filtrationFiltration and half evaporation
7. customgave a white suspension which
8. filtrationwas filtered off
9. washwashed with ether