Sulfuric Acid → 2,4-Dinitro-6-chlorobenzene-diazonium sulfate

HRID 127837

Reaktionsgleichung

Reaktionsgleichung von HRID 127837
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[N+:6]([C:9]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[C:12]([Cl:19])[C:10]=1[NH2:11])([O-:8])=[O:7].[N:20](OS(=O)(=O)O)=O>>[S:1]([O-:5])([O-:4])(=[O:3])=[O:2].[N+:6]([C:9]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[C:12]([Cl:19])[C:10]=1[N+:11]#[N:20])([O-:8])=[O:7].[N+:6]([C:9]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[C:12]([Cl:19])[C:10]=1[N+:11]#[N:20])([O-:8])=[O:7]

Komponenten

4

Edukt 3

HCID 1118Sulfuric AcidHCID 190526-Chloro-2,4-dinitroaniline2×HCID 82157Nitrosylsulfuric acid

Produkt 1

HCID 234700412,4-Dinitro-6-chlorobenzene-diazonium sulfate

Versuchsvorschrift

1000 Parts by weight of 100% sulfuric acid are placed into a stirring flask. 217.5 Parts by weight of 100% 2,4-dinitro-6-chloroaniline are then introduced in a way that the temperature of 40° C. is not exceeded. After the entire 2,4-dinitro-6-chloroaniline has been dissolved, 334 parts by weight of 40% nitrosyl-sulfuric acid are introduced, starting at a temperature of from 20° to 25° C., in such a manner that the temperature rises by itself to 35° to 38° C. Subsequently the mixture is continued to be stirred for 2 hours. A test is made to find out whether a sample is clearly soluble in ice water. After the diazotization has been completed, the mixture is cooled to +20° C., and the solution thus obtained of 2,4-dinitro-6-chlorobenzene-diazonium sulfate is added to an agitated mixture of 1500 parts by weight of water, 2000 parts by weight of ice, 224 parts by weight of 2-amino-4-acetamino-1-β-methoxy-ethoxy-benzene and 100 parts by weight of acetic acid within 30 minutes. During the addition process the temperature is maintained at 0° C. by adding about 3000 parts by weight of ice. Stirring is continued for 30 minutes, then the mixture is diluted with 6000 parts by weight of water and stirred for another hour. Finally the dyestuff formed is filtered off and washed with water until it is free from acid.

Aufarbeitung

  1. customstarting at a temperature of from 20° to 25° C.
  2. customrises by itself to 35° to 38° C
  3. temperaturethe mixture is cooled to +20° C.

Quellen und Nachweise

ORD-Eintrag
ord-249de5652fc9405e90abd02f0d8765c7
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04257943

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