反应详情

A mixture of 4.4 parts of 6-(2-bromoethyl)-2,3-dihydro-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one monohydrobromide, 3.7 parts of 6-fluoro-3-(4-piperidinyl)-1H-indazole dihydrochloride, 4.25 parts of sodium carbonate and 120 parts of 4-methyl-2-pentanone was stirred for 6 hours at reflux temperature. After cooling, the reaction mixture was filtered, The precipitate was stirred in water and the whole was filtered again. The precipitated product was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 2.5 parts (48.3%) of 6-[2-[4-(6-fluoro-1H-indazol-3-yl)-1-piperidinyl]ethyl]-2,3-dihydro-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one; mp. 207.6° C. (compound 2).

1. temperatureat reflux temperature
2. temperatureAfter cooling
3. filtrationthe reaction mixture was filtered
4. stirringThe precipitate was stirred in water
5. filtrationthe whole was filtered again
6. customThe precipitated product was purified by column chromatography over silica gel using
7. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
8. customThe pure fractions were collected
9. customthe eluent was evaporated
10. customThe residue was crystallized from 2-propanol
11. filtrationThe product was filtered off
12. customdried