Reaktion #548524

Reaktionsgleichung

methylvinylketon

HCl

10-keto-10,11-dihydrodibenzo(b,f)-oxepine

sodiumethoxide

→

2-keto-1,2,3,4-tetrahydro-tribenzo(b,d,f)-oxepine

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONare added, whereupon the solution
2. 2
   Temperaturis refluxed for 1 hour
3. 3
   TemperaturThe solution is cooled
4. 4
   ExtraktionAfter extracting into ether
5. 5
   Waschenwashing the ether layer with water (till neutral)
6. 6
   Sonstigedrying the etherial phase
7. 7
   Sonstigethe solvent is evaporated

Vorschrift

To a solution of 42 g of the compound 10-keto-10,11-dihydrodibenzo(b,f)-oxepine in 200 ml of dry ethanol a solution of sodiumethoxide (7 g of sodium in 500 ml of ethanol) is added dropwise. After stirring the mixture for 30 minutes 16.2 ml of methylvinylketon in 50 ml of ethanol are added, whereupon the solution is refluxed for 1 hour. The solution is cooled then and poured into 2 N HCl. After extracting into ether, washing the ether layer with water (till neutral) and drying the etherial phase, the solvent is evaporated.

Quelle