Ammonium Chloride → 2,6-Difluoropyridin-3-amine

Temperature

80 °C

2,6-Difluoro-3-nitropyridine (3.84 g) was dissolved in ethanol (42 ml). A solution of iron powder (4.03 g) and ammonium chloride (2.57 g) in water (14 ml) was added, and the reaction solution was heated and stirred at 80° C. for one hour. After leaving to cool, the reaction solution was filtered through celite. Ethyl acetate and water were added and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.06 g). The property values of the compound are as follows.

1. temperaturethe reaction solution was heated
2. customAfter leaving
3. temperatureto cool
4. filtrationthe reaction solution was filtered through celite
5. additionEthyl acetate and water were added
6. customthe organic layer was separated
7. washThe resulting organic layer was washed with brine
8. dry with materialdried over anhydrous sodium sulfate
9. customThe drying agent was separated by filtration
10. concentrationthe organic layer was concentrated under reduced pressure
11. customThe residue was purified by silica gel column chromatography

ORD record

ord-4c05e09ebfeb4a75b4e4a7fd2b7c68ce

Source dataset

uspto-grants-2011_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07935815B2