反应详情

温度

0 °C

Ethyl chloroformate (0.64 mL, 6.7 mmol) was added dropwise to a solution of 2-adamantyl-4-methylphenol (1.09 g, 4.5 mmol), Et3N (1.25 mL, 9 mmol) and DMAP (catalytic amount) in dichloromethane (8 mL) cooled in an ice-water bath to 0° C. The mixture was allowed to warm to room temperature while stirring overnight, then filtered and the filtrate was concentrated. The residue was purified by column chromatography (10-20% ethyl acetate-hexanes) to yield 2-admantyl-4-methyl-phenyl ethyl carbonate as a yellow oil (1.32 g, 94%).

1. temperatureto warm to room temperature
2. filtrationfiltered
3. concentrationthe filtrate was concentrated
4. customThe residue was purified by column chromatography (10-20% ethyl acetate-hexanes)