2,4-Dichloro-6-methyl-3-nitropyridine → 2,4-Dichloro-6-methylpyridin-3-amine

Temperature

60 °C

2,4-Dichloro-6-methyl-3-nitropyridine (30 g, 144.9 mmol) was dissolved in ethanol (300 mL), and Raney nickel (1.50 g, 25.6 mmol) was added to the solution, followed by stirring for 7 hours at 60° C. under hydrogen atmosphere (0.15 MPa). Raney nickel was removed through filtration, and the filtrate was concentrated under reduced pressure. The residue was dissolved in chloroform (60 mL), and the solution was left to stand for one hour. Subsequently, the formed insoluble substance was removed through filtration, and the filtrate was concentrated under reduced pressure, to thereby yield 24.62 g of 3-amino-2,4-dichloro-6-methylpyridine (yield: 96%) as a colorless solid. The product was recrystallized from hexane, to thereby yield colorless crystals.

1. customRaney nickel was removed through filtration
2. concentrationthe filtrate was concentrated under reduced pressure
3. dissolutionThe residue was dissolved in chloroform (60 mL)
4. waitthe solution was left
5. waitto stand for one hour
6. customSubsequently, the formed insoluble substance was removed through filtration
7. concentrationthe filtrate was concentrated under reduced pressure

ORD record

ord-345b2f5cb4c9400ab6148f1e4a730df3

Source dataset

uspto-grants-2007_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07176306B2