반응 #68414

반응 방정식

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

용매

MeOH

반응 조건

후처리

1. 1
   기타To a Parr reaction bottle
2. 2
   여과filtered
3. 3
   농축concentrated
4. 4
   추출extracted with EtOAc (×3)
5. 5
   세척The combined organic layer was washed with brine
6. 6
   건조dried over Na2SO4
7. 7
   농축concentrated in vacuo
8. 8
   workup.DISTILLATIONThe crude product was purified by distillation under vacuum

실험 절차

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.

출처