反应详情

温度

0 °C

Under argon atmosphere, to a solution of 3-(2,4-dimethoxybenzyl)-4-oxo-3-azabicyclo[3.1.0]hexane-1-carbaldehyde (10.8 mg) in tert-butanol/tetrahydrofuran/water (4/3/1, 0.5 ml) was added sodium dihydrogenphosphate dihydrate (20.2 mg) at room temperature. This reaction mixture was cooled to 0° C., 2-methyl-2-butene (18 μl) and sodium chlorite (9.0 mg) were sequentially added thereto, and then the mixture was stirred at room temperature for 24 hours. This reaction mixture was cooled to 0° C., and then water was added thereto, and the mixture was extracted with ethyl acetate. This organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel thin-layer chromatography (eluent: chloroform/methanol=9/1) to give the titled compound (3.7 mg).

1. temperatureThis reaction mixture was cooled to 0° C.
2. extractionthe mixture was extracted with ethyl acetate
3. washThis organic layer was washed with a saturated aqueous solution of sodium chloride
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by silica gel thin-layer chromatography (eluent: chloroform/methanol=9/1)