反应详情

A solution (15 ml) of 3.98 g of 1-benzyl-3-methyl-4-piperidone in diethyl ether was added to a suspension (10 ml) of 0.78 g of aluminum lithium hydride in diethyl ether in an ice bath, and the solution was heated under ref lux for 3 hours. Water was added to the solution, and the solution was extracted with ethyl acetate, and the organic layer was washed with saturated aqueous solution of hydrogen chloride. The solution was dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified with silica gel column chromatography, and from the fractions eluted with chloroform-methanol (19:1 v/v) was obtained 2.76 g of 1-benzyl-4-hydroxy-3-methylpiperidine, which was an oily product (yield: 69%).

1. temperaturethe solution was heated under ref lux for 3 hours
2. extractionthe solution was extracted with ethyl acetate
3. washthe organic layer was washed with saturated aqueous solution of hydrogen chloride
4. dry with materialThe solution was dried with anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified with silica gel column chromatography
7. washfrom the fractions eluted with chloroform-methanol (19:1 v/v)