反应详情

A mixture of 9.3 parts of 6-(2-bromoethyl)-3,7-dimethyl-5H-thiazolo[3,2-a]pyrimidin-5-one monohydrobromide, 6.5 parts of 4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]piperidine, 10.2 parts of sodium carbonate and 120 parts of 4-methyl-2-pentanone was stirred and refluxed overnight. The reaction mixture was cooled and water was added. 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 (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2,2'-oxybispropane. The product was filtered off and dried, yielding 4 parts (35%) of 6-[2-[4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-1-piperidinyl]ethyl]-3,7-dimethyl-5H-thiazolo[3,2-a]pyrimidin-5-one; mp. 140° C. (compound 35).

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 (98:2 by volume) as eluent
9. customThe pure fractions were collected
10. customthe eluent was evaporated
11. customThe residue was crystallized from 2,2'-oxybispropane
12. filtrationThe product was filtered off
13. customdried