Ammonium Chloride → HCID 66613369, Verbindung

HRID 406574

Reaktionsgleichung

Reaktionsgleichung von HRID 406574
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH3:15])[C:10]=1[N+:16]([O-])=O.[Cl-].[NH4+]>C(O)C.C(OCC)(=O)C.[Fe]>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH3:15])[C:10]=1[NH2:16]

Komponenten

6

Edukt 2

HCID 25517Ammonium ChlorideHCID 666141515-(2-chloro-4-fluorophenyl)-1,3-dimethyl-4-nitro-1H-pyrazole2×

Produkt 1

HCID 66613369HCID 66613369, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23925IronKatalysatorHCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-4-nitro-1H-pyrazole (i.e. the product of Step A) (0.2 g, 0.74 mmol), iron powder (0.2 g, 3.6 mmol) and saturated aqueous ammonium chloride solution (1 mL) in ethanol (5 mL) was heated at 80° C. for 4 h. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and filtered through a pad of Celite® (diatomaceous earth) on a sintered glass frit funnel. The filtrate was concentrated under reduced pressure and the resulting material was purified by silica gel column chromatography (ethyl acetate as eluant) to provide the title compound (0.14 g).

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. filtrationfiltered through a pad of Celite® (diatomaceous earth) on a sintered glass frit funnel
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe resulting material was purified by silica gel column chromatography (ethyl acetate as eluant)

Quellen und Nachweise

ORD-Eintrag
ord-72847333c3c34584999175d34cdd44cc
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08754115B2

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