반응 #95326

반응 방정식

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

수율 93.0%

용매

methanol

methanol

반응 조건

후처리

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

실험 절차

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.

출처