Ammonium Chloride → HCID 67974925, Verbindung

HRID 706655Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 706655
[CH2:1]([O:3][C:4]1[N:9]=[C:8]([CH2:10][N:11]2[C:19]3[C:14](=[C:15]([N+:20]([O-])=O)[CH:16]=[CH:17][CH:18]=3)[C:13]([CH3:23])=[N:12]2)[CH:7]=[CH:6][CH:5]=1)[CH3:2].[Cl-].[NH4+]>[Fe].CCO.O>[CH2:1]([O:3][C:4]1[N:9]=[C:8]([CH2:10][N:11]2[C:19]3[CH:18]=[CH:17][CH:16]=[C:15]([NH2:20])[C:14]=3[C:13]([CH3:23])=[N:12]2)[CH:7]=[CH:6][CH:5]=1)[CH3:2]

Komponenten

5

Edukt 2

HCID 25517Ammonium ChlorideHCID 67976364HCID 67976364, Verbindung

Produkt 1

HCID 67974925HCID 67974925, VerbindungAusbeute 71,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 19096565Water ethanolLösungsmittel

Versuchsvorschrift

A solution of 1-((6-ethoxypyridin-2-yl)methyl)-3-methyl-4-nitro-1H-indazole (0.118 g, 0.378 mmol), ammonium chloride (0.0101 g, 0.189 mmol) in 4:1 EtOH/water (2 mL) was treated with iron (0.211 g, 3.78 mmol) and refluxed for 2 hours. The solvent was removed and the residue taken in EtOAc-water and filtered through glass fiber filter paper. The organic phase was separated, dried (phase separator silicone treated filter paper), and concentrated to provide 1-((6-ethoxypyridin-2-yl)methyl)-3-methyl-1H-indazol-4-amine (0.076 g, 71% yield) as a yellow gum.

Aufarbeitung

  1. temperaturerefluxed for 2 hours
  2. customThe solvent was removed
  3. filtrationfiltered through glass fiber
  4. filtrationfilter paper
  5. customThe organic phase was separated
  6. customdried
  7. addition(phase separator silicone treated filter paper)
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-1f317b418c6a499e865a443c815d7e6b
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09174981B2

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