反应详情

温度

50 °C

To a mixed solution of methyl 2-[4-({4′-[(1,1-dioxidotetrahydro-2H-thiopyran-4-yl)oxy]-2′,6′- dimethylbiphenyl-3-yl}methoxy)phenyl]cyclopropanecarboxYlate (0.392 g, 0.733 mmol) in methanol (6 mL) and tetrahydrofuran (12 mL) was added 2 M aqueous sodium hydroxide solution (3 mL), and the mixture was stirred at 50° C. for 2 hr. 1 M Hydrochloric acid (10 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=50:50-90:10) and recrystallized from ethyl acetate-hexane to give the title compound (0.129 g, yield 34%) as colorless crystals.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=50:50-90:10)
6. customrecrystallized from ethyl acetate-hexane