反应详情

温度

70 °C

A sealed tube was charged with 139a (2.145 g, 15 mmol), Cs2CO3 (978 mg, 3.0 mmol), and 2,2-dimethyloxirane (15 mL). The mixture was stirred at 70° C. for 3 h. After cooled to room temperature, the mixture was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with petroleum ether/ethyl acetate (5:1 to 1:1) to afford 139b (1.2 g, 38%) as a white solid. MS-ESI: [M+H]+ 216.2

1. temperatureAfter cooled to room temperature
2. concentrationthe mixture was concentrated under reduced pressure
3. customThe residue was purified by silica-gel column chromatography
4. washeluting with petroleum ether/ethyl acetate (5:1 to 1:1)