反应详情

A mixture of 7.4 parts of 7-(2-bromoethyl)-3,4-dihydro-8-methyl-2H, 6H-pyrimido[2,1-b][1,3]thiazin-6-one monohydrobromide, 6.6 parts of 4-(diphenylmethylene)piperidine hydrobromide, 12 parts of sodium carbonate and 120 parts of 4-methyl-2-pentanone was stirred and refluxed overnight. The reaction mixture was cooled, water was added and the layers were separated. The organic phase 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 crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product was filtered off and recrystallized from 2-propanol, yielding 5.5 parts (60%) of 7-[2-[4-(diphenylmethylene)-1-piperidinyl]ethyl]-3,4-dihydro-8-methyl-2H,6H-pyrimido[2,1-b][1,3]-thiazin-6-one; mp. 176.0° C. (compound 104).

1. temperaturerefluxed overnight
2. temperatureThe reaction mixture was cooled
3. customthe layers were separated
4. customThe organic phase 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. customThe residue was crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
12. filtrationThe product was filtered off
13. customrecrystallized from 2-propanol