반응 #997754

반응 방정식

2-Methylglutaronitrile

NH3

→

3-methylpyridine-2,6-diamine

용매

반응 조건

후처리

1. 1
   온도The mixture was cooled to ambient temperature
2. 2
   기타the excess NH3 removed by N2
3. 3
   기타purge
4. 4
   기타the catalyst was removed by syringe
5. 5
   여과filtration
6. 6
   기타the crude reaction mixture
7. 7
   농축was concentrated in vacuo

실험 절차

2-Methylglutaronitrile was combined with Pd.C (5 mol % of 10 wt % Pd on carbon) in a 10 mL Hastelloy shaker autoclave to which liquid NH3 was added. The mixture was heated at 200° C. for 45 h. The mixture was cooled to ambient temperature and the excess NH3 removed by N2 purge. The crude mixture was suspended in 10 mL anhydrous methanol, the catalyst was removed by syringe filtration, and the crude reaction mixture was concentrated in vacuo. 2-Methylglutaronitrile conversion was 100% to give 0.02 mmol of 3-methylpyridine-2,6-diamine in 2.3% net yield.

출처