Methylamine → 2,6-Dichloro-N-methylpyridin-4-amine

Temperatur

57.5 °C

An 8M solution of methylamine in ethanol (5 ml; 40 mmol) was added drop wise to a stirred solution of 2,4,6-trichloropyridine (5 g; 27.4 mmol) in absolute ethanol (50 ml). After heating to 55-60° C. for 24 hr, the mixture was cooled to rt and concentrated. After adding water (50 ml) to the residue, the resulting suspension was filtered and the white filter cake was washed with water (3×10 ml). After air drying, the solid was suspended in dichloromethane (25 ml) and stirred for 10 minutes. Filtration, rinsing with dichloromethane and drying afforded 2.45 g (51%) of A1.6 as a white solid. HPLC (A): 95%, ret. time=1.16 min., LC/MS (M+H)+=177.00 (178.99).

1. temperaturethe mixture was cooled to rt
2. concentrationconcentrated
3. additionAfter adding water (50 ml) to the residue
4. filtrationthe resulting suspension was filtered
5. washthe white filter cake was washed with water (3×10 ml)
6. customAfter air drying
7. filtrationFiltration
8. washrinsing with dichloromethane
9. customdrying
10. customafforded 2.45 g (51%) of A1.6 as a white solid

ORD-Eintrag

ord-272212491dca4f0c92f071200cef1acb

Quelldatensatz

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07557211B2