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

HRID 1087992

Reaktionsgleichung

Reaktionsgleichung von HRID 1087992
[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(NC=NCCCC)CCC.[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 86744256HCID 86744256, VerbindungHCID 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), 2.3 g of N,N'-dibutylformamidine 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, 97% 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-45196dd3922c46828428291de1cdc84c
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04960936

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