反应详情

A mixture of 2.5 parts of 3-[2-[4-[(2-fluorophenyl)(2-phenylhydrazono)methyl]-1-piperazinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, 1 part of potassium carbonate and 27.8 parts of 1,2-ethanediol was stirred overnight at reflux temperature. The reaction mixture was cooled and then poured into water. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in 2-propanol. The salt was filtered off and dried, yielding 0.7 parts (25.5%) of 2-methyl-3-[2-[4-(1-phenyl-1H-indazol-3-yl)-1-piperazinyl]ethyl]-4H-pyrido[1,2-a]pyrimidin-4-one; mp. 260.0° C. (decomp.) (compound 4).

1. temperatureat reflux temperature
2. temperatureThe reaction mixture was cooled
3. extractionThe product was extracted with dichloromethane
4. customThe extract was dried
5. filtrationfiltered
6. customevaporated
7. customThe residue was 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 were collected
10. customthe eluent was evaporated
11. filtrationThe salt was filtered off
12. customdried