反应详情

To 50 mg of 2-acetylnicotinic acid are added 56 mg of 4-(3,5-difluorophenyl)semicarbazide and 1 mL of methanol. After a minute of stirring the product begins precipitating from the solution. After stirring overnight (15 h) the stir vane is removed and rinsed with 0.2 mL of methanol. The reaction mixture is centrifuged and the supernatant solution removed. In the same way the solid is rinsed with methanol (3×0.5 mL) and ether (1×0.5 mL). The solid is dried in vacuo with heating to give 2-acetylnicotinic acid 4-(3,5-difluorophenyl)semicarbazone (also known as 2-[methyl-{[(3,5-difluorophenylamino)carbonyl]hydrazono}methyl]-3-pyridine-carboxylic acid), m.p. 186° (compound 31, Table A).

1. custombegins precipitating from the solution
2. stirringAfter stirring overnight (15 h) the stir vane
3. customis removed
4. washrinsed with 0.2 mL of methanol
5. customthe supernatant solution removed
6. washIn the same way the solid is rinsed with methanol (3×0.5 mL) and ether (1×0.5 mL)
7. customThe solid is dried in vacuo
8. temperaturewith heating