反应详情

To a solution of 3-bromofuran-2-carbaldehyde (25.0 g) and 2-methyl-2-butene (45.4 mL) in tert-butanol (250 mL) was added dropwise a solution of 80% sodium chlorite (40.5 g) and sodium dihydrogen phosphate (51.5 g) in water (350 mL) at room temperature, and the mixture was stirred overnight. To the reaction mixture was added 1M hydrochloric acid (300 ml), 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 washed with hexane/ethyl acetate (5/1) and recrystallized from hexane/ethyl acetate to give the title compound (20.3 g). 1H NMR (300 MHz, CDCl3) δ 6.66 (1H, d, J=1.9 Hz), 7.58 (1H, d, J=1.9 Hz).

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. washThe residue was washed with hexane/ethyl acetate (5/1)
6. customrecrystallized from hexane/ethyl acetate