反应详情

A 100-mL round-bottomed flask equipped with a reflux condenser was charged with 150f (2.0 g, 1.0 eq., 6.4 mmol), K2CO3 (1.77 g, 2.0 eq., 12.8 mmol), acetonitrile (50 mL). The reaction mixture was reflux overnight. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 4:1 petroleum ether/ethyl acetate to afford 150g (550 mg, 37%, over two steps) as a colorless oil. MS-ESI: [M+H]+ 232.3

1. customA 100-mL round-bottomed flask equipped with a reflux condenser
2. temperatureThe reaction mixture was reflux overnight
3. filtrationfiltered
4. concentrationThe filtrate was concentrated under reduced pressure
5. customThe residue was purified by silica-gel column chromatography
6. washeluting with 4:1 petroleum ether/ethyl acetate