反应详情

A mixture of 5 parts of 3-(2-chloroethyl)-2-methyl-4H-pyrido-[1,2-a]pyrimidin-4-one, 4.9 parts of (4-fluorophenyl)(4-piperidinyl)-methanone hydrochloride, 5 parts of sodium carbonate and 160 parts of 4-methyl-2-pentanone is stirred and refluxed for 24 hours. The reaction mixture is cooled, washed with water and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (92:8 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 3 parts of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one; mp. 139° C.

1. temperaturerefluxed for 24 hours
2. temperatureThe reaction mixture is cooled
3. washwashed with water
4. customthe layers are separated
5. customThe organic phase is dried
6. filtrationfiltered
7. customevaporated
8. customThe residue is purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (92:8 by volume) as eluent
10. customThe pure fractions are collected
11. customthe eluent is evaporated
12. customThe residue is crystallized from a mixture of ethanol and 1,1'-oxybisethane