Reaktion #95326

Reaktionsgleichung

disodium

(24R)-22ξ-phenylsulfonyl-5,7-cholestadiene-3β,24,25-triol 3-tetrahydropyranyl ether

→

(24R)-5,7-cholestadiene-3β,24,25-triol 3-tetrahydropyranyl ether

Ausbeute 93.0%

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred for 30 minutes at room temperature
2. 2
   Filtrationthe precipitate was filtered
3. 3
   SonstigeThe filtrate was evaporated under reduced pressure
4. 4
   Extraktionthe residue was extracted with ethyl acetate
5. 5
   WaschenThe organic layer was washed with saturated brine
6. 6
   Trocknendried over anhydous sodium sulfate
7. 7
   SonstigeThe solvent was evaporated under reduced pressure

Vorschrift

A mixture of 1 g of anhydrous disodium hydrogenephosphate and 3.2 g of 5% sodium-amalgam was added to a solution of 160 mg of (24R)-22ξ-phenylsulfonyl-5,7-cholestadiene-3β,24,25-triol 3-tetrahydropyranyl ether in 5 ml of methanol in an argon stream under stirring, and the mixture was stirred for 30 minutes at room temperature. To the reaction mixture 10 ml of methanol was added and the precipitate was filtered. The filtrate was evaporated under reduced pressure and the residue was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydous sodium sulfate. The solvent was evaporated under reduced pressure to give 11.6 mg (93%) of (24R)-5,7-cholestadiene-3β,24,25-triol 3-tetrahydropyranyl ether.

Quelle