Hydrochloric Acid → 2-Chloropyridine-3,5-diamine

Temperature

80 °C

The mixture of 2.19 g of iron powder, 5 ml of water, and 10 ml of ethanol was stirred at 80° C. for 2 minutes. After incremental addition of 1 ml concentrated hydrochloric acid, the mixture was stirred at the same temperature until the solution became neutral. To the reaction solution was incrementally added suspension of 1 g 2-chloro-3,5-dinitropyridine in 5 ml ethanol, and the mixture was stirred at 80° C. for 40 minutes. The reaction solution was allowed to cool, and the iron was removed by filtration with celite, and the solvent of the filtrate was distilled off. Ethanol was added to the residue to disperse the solid content, and the solid content was collected by filtration to obtain 360 mg of the title compound.

1. stirringthe mixture was stirred at the same temperature until the solution
2. stirringthe mixture was stirred at 80° C. for 40 minutes
3. temperatureto cool
4. customthe iron was removed by filtration with celite
5. distillationthe solvent of the filtrate was distilled off
6. additionEthanol was added to the residue
7. additionto disperse the solid content
8. filtrationthe solid content was collected by filtration

ORD record

ord-3725e5f81f544f39ab1f600396823549

Source dataset

uspto-grants-2000_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06133284