反应详情

To a cold stirred mixture of 8.75 g (0.039 mole) of methyl 2,6-dichloronicotinate N-oxide in 50 ml of methanol was added dropwise 2.0 g (0.063 mole) of hydrazine in 14 ml of methanol. After complete addition the mixture was stirred for one hour then placed in a freezer for approximately 18 hours. The solvent was then removed by distillation under reduced pressure to leave a solid. The solid was stirred in isopropanol then filtered. The filter cake was added to 75 ml of refluxing ethanol and the resulting mixture filtered hot to yield 4.3 g of 2,6-dichloro-4-pyridinecarboxylic acid hydrazide 1-oxide as a solid.

1. additionAfter complete addition the mixture
2. stirringwas stirred for one hour
3. customThe solvent was then removed by distillation under reduced pressure
4. customto leave a solid
5. filtrationthen filtered
6. additionThe filter cake was added to 75 ml of refluxing ethanol
7. filtrationthe resulting mixture filtered hot