反应详情

A mixture of 88.8 parts of ethyl 4-[[[(4-amino-6-hydroxy-5-pyrimidinyl)[(4-fluorophenyl)methyl]amino]thioxomethyl]amino]-1-piperidinecarboxylate, 88 parts of mercury(II) oxide, 0.1 parts of sulfur and 1200 parts of ethanol was stirred overnight at reflux temperature. The reaction mixture was filtered over diatomaceous earth while hot and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from ethyl acetate. The product was filtered off and dried, yielding 50.7 parts (66.1%) of ethyl 4-[[7-amino-1-[(4-fluorophenyl)methyl]oxazolo[5,4-d]-pyrimidin-2(1H)-yliden]amino]-1-piperidinecarboxylate; mp. 174.6° C. (compound 24).

1. temperatureat reflux temperature
2. filtrationThe reaction mixture was filtered over diatomaceous earth while hot and the filtrate
3. customwas evaporated
4. customThe residue was purified by column chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol
6. customThe pure fractions were collected
7. customthe eluent was evaporated
8. customThe residue was crystallized from ethyl acetate
9. filtrationThe product was filtered off
10. customdried