反应详情

A mixture of 5.6 parts of 1-(3-chloropropyl)-2,3-dihydro-2,2-dimethyl-4(1H)-quinazolinone, 4.9 parts of (4-fluorophenyl) (4-piperidinyl)methanone hydrochloride, 10 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled, water is added and the layers are separated. The 4-methyl-2-pentanone phase is dried, filtered and evaporated. The solid 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 solid residue is stirred in 2,2'-oxybispropane. The product is filtered off and dried, yielding 6.6 parts (78%) of 1-[3-[4-(4-fluorobenzoyl)-1-piperidinyl]propyl]-2,3-dihydro-2,2-dimethyl-4(1H)-quinazolinone; mp. 185.7° C.

1. temperatureThe reaction mixture is cooled
2. customthe layers are separated
3. dry with materialThe 4-methyl-2-pentanone phase is dried
4. filtrationfiltered
5. customevaporated
6. customThe solid residue is purified by column-chromatography over silica gel using
7. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
8. customThe pure fractions are collected
9. customthe eluent is evaporated
10. stirringThe solid residue is stirred in 2,2'-oxybispropane
11. filtrationThe product is filtered off
12. customdried