反应详情

A mixture of 2 g (6.1 mmol) 1-[(3S,4S)-1-Benzyl-3-(4-chloro-phenyl)-piperidin-4-yl]-ethanone, 0.869 g (12.5 mmol) hydroxylamine, hydrochloride and 1.03 g (12.5 mmol) sodium acetate in 25 mL ethanol was heated to reflux for 2 h. After cooling to room temperature water was added and the mixture was extracted with ethyl acetate. The combined organic phases were dried with Na2SO4, filtered and evaporated to dryness. The residue was purified by flash column chromatography on silica eluting with a ethyl acetate. The product containing fractions were evaporated to yield 1.6 g (77%) of the title compound as colorless viscous oil. MS (m/e): 343.2 [(M+H)+].

1. temperaturewas heated
2. temperatureto reflux for 2 h
3. additionwas added
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe combined organic phases were dried with Na2SO4
6. filtrationfiltered
7. customevaporated to dryness
8. customThe residue was purified by flash column chromatography on silica eluting with a ethyl acetate
9. additionThe product containing fractions
10. customwere evaporated