반응 #68413

반응 방정식

HCl

2,6-dichloro-5-fluoronicotinonitrile

→

title compound

(2,6-Dichloro-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
   workup.DISSOLUTIONThe crude was dissolved in EtOAc
5. 5
   기타the layers were separated
6. 6
   세척The organic layer was washed with brine
7. 7
   건조dried over Na2SO4
8. 8
   농축concentrated in vacuo

실험 절차

To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 6 M HCl (50 ml) and a solution of 2,6-dichloro-5-fluoronicotinonitrile (Aldrich, 10.0 g, 52.4 mmol) in MeOH (100 ml). The mixture was placed under 50 psi H2 on a shaker type Parr apparatus for 21 h, filtered and concentrated. The crude was dissolved in EtOAc, basified with aqueous NaOH, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo to yield the title compound as crude light yellow oil. Used without further purification.

출처