Hydrochloric Acid → 5-Iodopyridine-2,3-diamine

HRID 1434636

Reaktionsgleichung

Reaktionsgleichung von HRID 1434636
[I:1][C:2]1[CH:3]=[C:4]([N+:9]([O-])=O)[C:5]([NH2:8])=[N:6][CH:7]=1.C(O)C.Cl>[Fe].O>[I:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:8])=[N:6][CH:7]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 33844682-Amino-5-iodo-3-nitropyridine

Produkt 1

HCID 218827665-Iodopyridine-2,3-diamineAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

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).

Aufarbeitung

  1. customThe iron was then removed
  2. washwashed with ethanol over
  3. filtrationa flitted filter while the ethanol washings
  4. concentrationwere concentrated under reduced pressure
  5. customThe residue was purified by flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-4a27429fc4e14527be8693d1c860e8c4
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07615567B2

Verknüpfte Notizen

Wird geladen…