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温度

0 °C

A round-bottomed flask was charged with 231a (600 mg, 1.72 mmol), dichloromethane (50 mL), and triethylamine (5 mL). The solution was stirred at 0° C. for 0.5 h and acetyl chloride (135 mg, 1.72 mmol) was added slowly. The mixture was stirred at 0° C. for another 2.5 h. It was then evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 9:1 petroleum ether/ethyl acetate to afford 231b (605 mg, 90%) as a yellow solid. MS-ESI: [M+H]+ 392.1

1. stirringThe mixture was stirred at 0° C. for another 2.5 h
2. customIt was then evaporated under reduced pressure
3. customThe residue was purified by silica-gel column chromatography
4. washeluting with 9:1 petroleum ether/ethyl acetate