Process for the continuous preparation of 3,3'-dichloro-benzidine dihydrochloride
AssigneeHoechst Aktiengesellschaft
InventorsKurt Habig, Konrad Baessler, Klaus Warning
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AssigneeHoechst Aktiengesellschaft
InventorsKurt Habig, Konrad Baessler, Klaus Warning
Estimating the term…
A process for the continuous preparation of 3,3'-dichlorobenzidine dihydrochloride from 2,2'-dichlorohydrazobenzene by treatment with aqueous sulfuric acid, which comprises treating the 2,2'-dichlorohydrazobenzene, dissolved in a water-immiscible aromatic solvent, continuously at temperatures of from about 20.degree. to about 50.degree. C. in the presence of an alkali metal salt of an alkyl (C.sub.8 -C.sub.23)polyglycol ether sulfate, with such an amount of from about 50 to about 80 % strength aqueous sulfuric acid that the suspension formed remains conveyable, subsequently diluting the suspension emerging from the reaction zone with water, again continuously, and subsequently heating the suspension to a temperature of from about 90.degree. to about 95.degree. C. until a solution is obtained, separating off the aromatic solvent from the hot, sulfuric acid aqueous phase, and precipitating the 3,3'-dichlorobenzidine dihydrochloride by adding hydrochloric acid to the sulfuric acid solution which remains and filtering off this product.
A process for the continuous preparation of 3,3'dichlorobenzidine dihydrochloride from 2,2'-dichlorohydrazobenzene by treatment with aqueous sulfuric acid, which comprises treating the 2,2'-dichlorohydrazobenzene, dissolved in a water-immiscible aromatic solvent, continuously at temperatures of from about 20.degree. to about 50.degree. C in the presence of an alkali metal salt of an alkyl (C.sub.8 -C.sub.23)polyglycol ether sulfate, with such an amount of from about 50 to about 80 % strength aqueous sulfuric acid that the suspension formed remains conveyable, subsequently diluting the suspension emerging from the reaction zone with water, again continuously, and subsequently heating the suspension to a temperature of from about 90.degree. to about 95.degree. C. until a solution is obtained, separating off the aromatic solvent from the hot, sulfuric acid aqueous phase, and precipitating the 3,3'-dichlorobenzidine dihydrochloride by adding hydrochloric acid to the sulfuric acid solution which remains, and filtering off this product.
A continuous process for the preparation of 3,3'-dichlorobenzidine dihydrochloride from 2,2'-dichlorohydrazobenzene by treatment with aqueous sulfuric acid, which comprises:
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