反应详情

The crude 1,4-dihydro-4-oxo-5-(phenylmethoxy)-2-pyridinecarboxylic acid, hydrazide, trifluoroacetate (1:2) salt was dissolved in 250 ml of acetonitrile and stirred with cooling for 1 hour. The crystals were then filtered off and resuspended in 600 ml of acetonitrile. Bis(trimethylsilyl)acetamide (135 ml) was added followed by 28 g of 10% palladium on charcoal. Then hydrogen was passed through the stirred solution. The hydrogenation was complete after 90 minutes. After filtration, 70 ml of methanol and 2 ml of acetic acid were added. After stirring overnight, the crystals formed were filtered off, yielding 19.4 g of the title compound, melting point 290°-340° C., dec.

1. temperaturewith cooling for 1 hour
2. filtrationThe crystals were then filtered off
3. additionBis(trimethylsilyl)acetamide (135 ml) was added
4. filtrationAfter filtration, 70 ml of methanol and 2 ml of acetic acid
5. additionwere added
6. stirringAfter stirring overnight
7. customthe crystals formed
8. filtrationwere filtered off