反应详情

A mixture of 5.6 parts of 3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, 6 parts of phenyl(4-piperidinyl)-methanone hydrobromide, 8 parts of sodium carbonate, 0.1 parts of potassium iodide and 240 parts of 4-methyl-2-pentanone is stirred and refluxed for 24 hours using a water-separator. The reaction mixture is filtered hot over Hyflo and the filtrate is evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from a mixture of ethanol and 1,1'-oxybisethane, yielding 6 parts of 3-[2-(4-benzoyl-1-piperidinyl)ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one; mp. 122.2° C.

1. temperaturerefluxed for 24 hours
2. filtrationThe reaction mixture is filtered hot over Hyflo
3. customthe filtrate is evaporated
4. customThe residue is purified by column-chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
6. customThe pure fractions are collected
7. customthe eluent is evaporated
8. customThe residue is crystallized from a mixture of ethanol and 1,1'-oxybisethane