Reaktion #68414

Reaktionsgleichung

NH3.H2O

(2,6-dichloro-5-fluoropyridin-3-yl)methanamine

Compound 144

(2,6-dichloro-5-fluoropyridin-3-yl)methanamine

→

title compound

(5-Fluoropyridin-3-yl)methanamine

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a Parr reaction bottle
2. 2
   Filtrationfiltered
3. 3
   Einengenconcentrated
4. 4
   Extraktionextracted with EtOAc (×3)
5. 5
   WaschenThe combined organic layer was washed with brine
6. 6
   Trocknendried over Na2SO4
7. 7
   Einengenconcentrated in vacuo
8. 8
   workup.DISTILLATIONThe crude product was purified by distillation under vacuum

Vorschrift

To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 28% NH3.H2O (50 ml) and a solution of (2,6-dichloro-5-fluoropyridin-3-yl)methanamine (Compound 144, 10.1 g, 52 mmol) in MeOH (100 ml). The mixture was placed under 51 psi H2 on a shaker type Parr apparatus for 16 h, filtered and concentrated. The resulting aqueous solution was basified with NaOH, extracted with EtOAc (×3). The combined organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The crude product was purified by distillation under vacuum to yield the title compound as colorless oil.

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