反应详情

To a stirred mixture of 20.9 parts of 1-(3-methylphenyl)-2-[1-(phenylmethyl)-4-piperidinyl]ethanone, 0.75 parts of sodium carbonate and 150 parts of trichloromethane are added dropwise 8.1 parts of ethyl chloroformate. Upon completion, stirring is continued overnight at room temperature. Water is added to the reaction mixture and the layers are separated. The aqueous phase is extracted with trichloromethane. The combined organic phases are washed with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 18 parts (91%) of ethyl 4-[2-(3-methylphenyl)-2-oxoethyl]-1-piperidinecarboxylate as an oily residue.

1. customthe layers are separated
2. extractionThe aqueous phase is extracted with trichloromethane
3. washThe combined organic phases are washed with water
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue is purified by column-chromatography over silica gel using
8. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
9. customThe pure fractions are collected
10. customthe eluent is evaporated