反应详情

A mixture of 8 parts of 6-(2-bromoethyl)-2,3-dihydro-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one monohydrobromide, 4.8 parts of 1-[(2,4-difluorophenyl)(hydroxyimino)methyl]piperazine, 8 parts of sodium hydrogen carbonate and 180 parts of 4-methyl-2-pentanone was stirred for 20 hours at reflux temperature. The reaction mixture was filtered while hot and the filtrate was evaporated in vacuo. 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 concentrated in vacuo. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 4.4 parts (50.5%) of 6-[2-[4-[(2,4-difluorophenyl)-(hydroxyimino)methyl]-1-piperazinyl]ethyl]-2,3-dihydro-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one (int. 13).

1. temperatureat reflux temperature
2. filtrationThe reaction mixture was filtered while hot and the filtrate
3. customwas evaporated in vacuo
4. customThe residue was purified by column chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
6. customThe pure fractions were collected
7. concentrationthe eluent was concentrated in vacuo
8. customThe residue was crystallized from acetonitrile
9. filtrationThe product was filtered off
10. customdried