Reaktion #1856734

Reaktionsgleichung

charcoal

Dibenzosuberenol

ethyl nitroacetate

diethyl ether

→

title compound

Ausbeute 41.3%

Ethyl α-nitro-5H-dibenzo-[a,d]cycloheptene-5-acetate

Ausbeute 41.3%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe oil bath is removed
2. 2
   Sonstigethe cooled reaction mixture
3. 3
   Filtrationfiltered
4. 4
   Temperaturcooled overnight
5. 5
   FiltrationA precipitate is collected by filtration
6. 6
   Waschenwashed with hexane, diethyl ether
7. 7
   Sonstigedried under vacuum at room temperature

Vorschrift

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.

Quelle