反应详情

温度

120 °C

Dibenzosuberenol (42 g, 0.2 mol) is combined with ethyl nitroacetate (25 mL, 0.23 mol) and the mixture is heated at 120° C. (oil bath) until melted and then kept at 110° C. for 2.5 hours. The oil bath is removed and the cooled reaction mixture is dissolved in 50 mL of methanol and taken up into 350 mL of boiling diethyl ether. The dark solution is treated with charcoal, filtered, and cooled overnight. A precipitate is collected by filtration, washed with hexane, diethyl ether, dried under vacuum at room temperature to give 26.7 g of the title compound; mp 101°-103° C.

1. customThe oil bath is removed
2. customthe cooled reaction mixture
3. filtrationfiltered
4. temperaturecooled overnight
5. filtrationA precipitate is collected by filtration
6. washwashed with hexane, diethyl ether
7. customdried under vacuum at room temperature