Reaktion #92986

Reaktionsgleichung

16β-ethyl-17β-bromoacetoxy-4-estren-3-one

potassium propionate

→

above-identified compound

Ausbeute 35.4%

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

Ausbeute 35.4%

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated under reduced pressure
2. 2
   ExtraktionThe residue is extracted with 200 ml of ethyl acetate
3. 3
   SonstigeThe organic layer is separated
4. 4
   Waschenwashed with water and saturated aqueous sodium chloride
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
7. 7
   Waschenpassage of 1000 ml isopropyl ether-n-hexane (2:3), elution
8. 8
   SonstigeThe eluate is evaporated under reduced pressure
9. 9
   Sonstigeto remove the solvent

Vorschrift

In a mixture of 50 ml of acetone and 12 ml of water are dissolved 2.5 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 0.7 g of potassium propionate. The solution is stirred at room temperature (17°-25° C.) for 3 days and concentrated under reduced pressure. 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 distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 1000 ml isopropyl ether-n-hexane (2:3), elution is carried out with 2000 ml of the same solvent system. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.87 g of the above-identified compound as white crystals.

Quelle