Methanol → 5-Chloro-3,6-difluoropyridin-2-amine

To 25 ml of methanol were added 2.7 g of 2-amino-4-bromo-5-chloro-3,6-difluoropyridine and 1.15 g of triethylamine together with 0.145 g of 10% palladium on carbon, and the mixture was hydrogenated at room temperature for 1.5 hours. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 50 ml of chloroform, and the mixture was washed with 30 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting colorless flake crystals were dispersed in a mixed solution of diisopropylether and n-hexane (1:2), and collected by filtration to obtain 1.62 g of the title compound.

1. customThe catalyst was separated by filtration
2. distillationthe solvent and the like were distilled off under reduced pressure
3. additionTo the residue was added 50 ml of chloroform
4. washthe mixture was washed with 30 ml of distilled water
5. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. additionThe resulting colorless flake crystals were dispersed in a mixed solution of diisopropylether and n-hexane (1:2)
8. filtrationcollected by filtration

ORD record

ord-137f4236c1554a50a52efc807d66773b

Source dataset

uspto-grants-2000_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06133284