HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylamine → N2,6-Dimethylpyridine-2,3-diamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylamine | HCID 6329 | — |
| Edukt | 2-Chloro-6-methyl-3-nitropyridine | HCID 1268230 | — |
| Edukt | HCID 178418361 | HCID 178418361 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | N2,6-Dimethylpyridine-2,3-diamine | HCID 22036951 | 83% |
Reaktionsschritte
2-Chloro-6-methyl-3-nitropyridine (2.5 g, 14.5 mmol) was stirred in 1.0 M solution of methylamine (40 ml, 40 mmol) in methanol at 70° C. for 60 min. After cooling to ambient temperature, and methanol (60 ml) and 10% palladium on activated carbon were added and the resulting mixture was shaken under 40 psi of hydrogen gas at ambient temperature for 30 min. The mixture was filtered through a pad of Celite and concentrated in vacuum. Chromatography on silica gel, eluting with a mixture dichloromethane-methanol-38% aqueous ammonia (9:1:0.1) yielded the title compound (1.65 g, 83%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07417041B2 |
| Quelldatensatz | uspto-grants-2008_08 |
| ORD ID | ord-d30ca6d1de0e4f2e917b81c522cca077 |
| Quellennotiz | uspto-grants-2008_08 |