Reaktion #313391

Reaktionsgleichung

methylamine

2,4,6-trichloropyridine

→

2,6-Dichloro-4-methylamino-pyridine

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was cooled to rt
2. 2
   Einengenconcentrated
3. 3
   workup.ADDITIONAfter adding water (50 ml) to the residue
4. 4
   Filtrationthe resulting suspension was filtered
5. 5
   Waschenthe white filter cake was washed with water (3×10 ml)
6. 6
   SonstigeAfter air drying
7. 7
   FiltrationFiltration
8. 8
   Waschenrinsing with dichloromethane
9. 9
   Sonstigedrying
10. 10
    Sonstigeafforded 2.45 g (51%) of A1.6 as a white solid

Vorschrift

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).

Quelle