Reaktion #92987

Reaktionsgleichung

16β-ethyl-bromoacetoxy-4-estren-3-one

potassium isobutyrate

→

above-identified compound

Ausbeute 70.8%

16β-Ethyl-17β-isobutyryloxyacetoxy-4-estren-3-one

Ausbeute 70.8%

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution is refluxed for 6 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
3. 3
   Extraktionthe residue is extracted with 200 ml of ethyl acetate
4. 4
   SonstigeThe organic layer is separated
5. 5
   Waschenwashed with water and saturated aqueous sodium chloride
6. 6
   Trocknendried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
8. 8
   Waschenpassage of 100 ml of diisopropyl ether, elution
9. 9
   SonstigeThe eluate is evaporated under reduced pressure
10. 10
    Sonstigeto remove the solvent

Vorschrift

In a mixture of 50 ml of acetone and 10 ml of water are dissolved 1.5 g of 16β-ethyl-bromoacetoxy-4-estren-3-one and 0.8 g of potassium isobutyrate and the solution is refluxed for 6 hours. The acetone is distilled off under reduced pressure and the residue is extracted with 200 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 100 ml of diisopropyl ether, elution is carried out with 300 ml of ethyl ether. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.08 g of the above-identified compound as a viscous oil.

Quelle