Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Ethanol | HCID 702 | — |
| Edukt | 2-Amino-5-iodo-3-nitropyridine | HCID 3384468 | — |
| Katalysator | Iron | HCID 23925 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 5-Iodopyridine-2,3-diamine | HCID 21882766 | 60% |
Reaktionsschritte
5-Iodo-3-nitro-2-aminopyridine (2.0 g, 7.55 mmol), ethanol (7 mL), water (2 mL), and concentrated HCl (0.10 mL) were added to a 25 mL round bottom flask and allowed to stir. Iron (4.8 g, 85.9 mmol) was added in portions to the reaction followed by heating at 100° C. for 30 min. The iron was then removed and washed with ethanol over a flitted filter while the ethanol washings were concentrated under reduced pressure. The residue was purified by flash chromatography using 1:2 hexane:ethyl acetate as eluent to give 5-Iodo-2,3-diaminopyridine as a light brown solid (60%, 1.061 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07615567B2 |
|---|
| Quelldatensatz | uspto-grants-2009_11 |
|---|
| ORD ID | ord-4a27429fc4e14527be8693d1c860e8c4 |
|---|
| Quellennotiz | uspto-grants-2009_11 |
|---|