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Published by: kanji63 on Nov 17, 2012
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11/17/2012

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Catalytic, reduction of 4,4'-dinitrodiphenylamine) 52 parts by weight (0.

2 mole) of 4,4'-dinitrodiphenylamine are reduced in 250 parts by weight of methanol and in the presence of 4 parts by weight of active carbon as well as 2 parts by weight of disodium hydrogen phosphate on 6 parts by weight of 5% nickel catalyst on active carbon (e.g. of the type RCH 55/5 from Ruhrchemie AG) in the course of 45 minutes at a hydrogen pressure of up to 40 bar and a temperature rising up to 140° C. On completion of the reduction, the catalyst is filtered from the reaction mixture whilst still hot and the filtrate stirred directly into about 400 parts by weight of about 5 % aqueous sulfuric acid. The mixture is stirred until cooled to about 20° C., and the product is filtered off with suction and washed with water. 54 parts by weight of 4,4'-diaminodiphenylamine sulfate are obtained, corresponding to a yield of 91% of theory. The sulfate salt can be converted to 4,4'-diaminodiphenylamine by treatment with aqueous alkali metal hydroxide .

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