反应详情

In a flask (50 ml) fitted with a condenser cholesterol 5α,6α-epoxide (100 mg., 0.25 mmol) in 1-propanol (20 ml) solution containing trifluoroacetic acid (1.0 ml) is refluxed for 1 hour. With vacuum evaporation the solvent is removed. The oily residue is dissolved in benzene (10 ml), extracted with 5% aqueous sodium bicarbonate (2 ml×2) and with water, and dried with anhydrous sodium sulfate. After vacuum evaporation the amorphous solid residue is purified by silica gel G-60 column liquid chromatography employing chloroform-methanol gradient elution. Selected fractions provide the product, 6β-n-propoxy-3β,5α-dihydroxycholestane. (45 mg).

1. temperatureis refluxed for 1 hour
2. customWith vacuum evaporation the solvent
3. customis removed
4. dissolutionThe oily residue is dissolved in benzene (10 ml)
5. extractionextracted with 5% aqueous sodium bicarbonate (2 ml×2) and with water
6. dry with materialdried with anhydrous sodium sulfate
7. customAfter vacuum evaporation the amorphous solid residue
8. customis purified by silica gel G-60 column liquid chromatography
9. washchloroform-methanol gradient elution