反应详情

A mixture of the above isothiourea salt (8.5 g, 27.0 mmol) and hydrazine (1.4 g, 27.0 mmol) in 80 ml of ethanol is heated to reflux for 4 hr. The mixture is cooled and the solvent removed. The residue is diluted with 80 ml of water and filtered. A 20 ml aliquot of the resulting aqueous filtrate (2.0 g, 11.9 mmol) is mixed with 2-acetylnicotinic acid (2.0 g, 11.9 mmol) in 6 ml of methanol and stirred at RT overnight. A bright yellow solid is collected by filtration and dried to give 2-[methyl(3-carboxy-2-pyridyl)methylene]-N-(3-fluorophenyl)hydrazinecarboximidamide, (compound 16).

1. temperatureis heated
2. temperatureto reflux for 4 hr
3. temperatureThe mixture is cooled
4. customthe solvent removed
5. additionThe residue is diluted with 80 ml of water
6. filtrationfiltered
7. filtrationA bright yellow solid is collected by filtration
8. customdried