反应详情

A mixture of 5.5 parts of 3-(2-chloroethyl)-2-phenyl-4(3H)-quinazolinone, 4 parts of (4-fluorophenyl)(4-piperidinyl)methanone hydrochloride, 7 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 24 hours using a water-separator. The reaction mixture is filtered while hot. The filtrate is 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. The residue is crystallized from a mixture of ethanol and 1,1'-oxybisethane. The product is filtered off and dried, yielding 5 parts (69%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2-phenyl-4(3H)-quinazolinone; mp. 143.8° C.

1. temperaturerefluxed for 24 hours
2. filtrationThe reaction mixture is filtered while hot
3. customThe filtrate is evaporated
4. customThe residue is purified by column-chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (95×5 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
9. filtrationThe product is filtered off
10. customdried