Water → Anilazine

HRID 2119203

Reaktionsgleichung

Reaktionsgleichung von HRID 2119203
[N:1]1[C:8]([Cl:9])=[N:7][C:5]([Cl:6])=[N:4][C:2]=1Cl.O.[Cl:11][C:12]1[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=1[NH2:14].[OH-].[Na+]>C1(C)C=CC=CC=1>[Cl:11][C:12]1[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=1[NH:14][C:2]1[N:1]=[C:8]([Cl:9])[N:7]=[C:5]([Cl:6])[N:4]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 72402-ChloroanilineHCID 7954Cyanuric chlorideHCID 14798Sodium Hydroxide

Produkt 1

HCID 7541AnilazineAusbeute 97,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

272.0 g of cyanuric chloride (content >99%), 1,000 ml of water and 275 ml of toluene are mixed at 5° C. The aqueous phase thereby assumes a pH value of 3.5. 188.2 g of o-chloroaniline are added in the course of 30 minutes without cooling or heating the mixture, whereupon the temperature rises to 30° C. A pH value of 7 is then established in the course of 1 hour by addition of 45% strength sodium hydroxide solution, whereupon the temperature rises up to 55° C. The mixture is then cooled to 20° C. in the course of 15 minutes. The product is filtered off, washed salt-free with water and dried at 60° C. in a waterpump vacuum. 396.5 g of 2-(2-chlorophenylamino)-4,6-dichloro-s-triazine are obtained with a melting point of 159° C. and a content of 98.9%, which corresponds to a yield of 97.5% (based on 99 % pure cyanuric chloride).

Aufarbeitung

  1. temperaturewithout cooling
  2. temperatureheating the mixture
  3. customrises to 30° C
  4. customrises up to 55° C
  5. filtrationThe product is filtered off
  6. washwashed salt-free with water
  7. customdried at 60° C. in a waterpump vacuum

Quellen und Nachweise

ORD-Eintrag
ord-2f1111996b854d52ae6d8b84a78706fc
Quelldatensatz
uspto-grants-1987_07
Patentnummer
US04683308

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