HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Chloro-2,4-Dinitrobenzene → 4-Chloro-M-phenylenediamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Chloro-2,4-Dinitrobenzene | HCID 6 | — |
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Cyanamide | HCID 9864 | — |
| Edukt | Formamidine acetate | HCID 160693 | — |
| Katalysator | Nickel | HCID 935 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 4-Chloro-M-phenylenediamine | HCID 21209 | — |
Reaktionsschritte
1.5 g of cyanamide, 1.5 g of acetic acid, 2 g of Raney nickel (60%, aqueous), and 120 ml of methanol are introduced in an autoclave equipped with gas introduction stirrer. Under a hydrogen pressure of 4 bar and a temperature of 25° C., the cyanamide is hydrogenated quantitatively to the formamidine acetate. 40.8 g of 1-chloro-2,4-dinitrobenzene are then added to the autoclave, and the hydrogenation is carried out at a pressure of 10 bar and a temperature of 60° C. The hydrogenation time is 1 hour. 1-Chloro-2,4-diaminobenzene, 97.5% pure (analysed as 1-Chloro-2,4-acetamidobenzene by liquid chromatography), is obtained in quantitative yield.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04960936 |
| Quelldatensatz | uspto-grants-1990_10 |
| ORD ID | ord-854f343b508f4d689cd02c64dc88fc11 |
| Quellennotiz | uspto-grants-1990_10 |