1-Chloro-2,4-Dinitrobenzene → 4-Chloro-M-phenylenediamine

HRID 1087988

Reaktionsgleichung

Reaktionsgleichung von HRID 1087988
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[N+:11]([O-])=O.C(O)(=O)C.C(N)=N.[H][H]>[Ni].CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][C:3]=1[NH2:11]

Komponenten

6

Edukt 3

HCID 61-Chloro-2,4-DinitrobenzeneHCID 160693Formamidine acetateHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 212094-Chloro-M-phenylenediamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

40.8 g of 1-chloro-2,4-dinitrobenzene, 2 g of Raney nickel (60%, aqueous), 1.5 g of formamidine acetate and 120 ml of methanol are introduced in an autoclave equipped with gas introduction stirrer. The air in the autoclave is then displaced by nitrogen and then by hydrogen. The hydrogenation is carried out at a pressure of 10 bar and a temperature of 60° C. The hydrogenation time is 11/4 hours. 1-Chloro-2,4-diaminobenzene, 99% pure (analysed as 1-Chloro-2,4-acetamidobenzene by liquid chromatography), is obtained in quantitative yield.

Aufarbeitung

  1. customequipped with gas introduction stirrer
  2. customa temperature of 60° C
  3. custom4 hours

Quellen und Nachweise

ORD-Eintrag
ord-559f18dcda8a431f96929c3468782f77
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04960936

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