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ChemicalBook CAS DataBase List 4-(PHENYLAZO)DIPHENYLAMINE
101-75-7

4-(PHENYLAZO)DIPHENYLAMINE synthesis

13synthesis methods
-

Yield:156-10-5 73.5% ，836-30-6 13.5% ，1227476-15-4 9.6% ，92-82-0 1.2% ，101-75-7 0.17%

Reaction Conditions:

potassium hydroxide;betaine in methanol;water at 40 - 80; under 30.003 - 150.015 Torr; for 6 h;

Steps:

20,21 xample 20 Batch Solution of the Reaction with Subsequent Processing of the Condensation Mixture, and Isolation of the 4-ADFA Product.

Example 20 Batch Solution of the Reaction with Subsequent Processing of the Condensation Mixture, and Isolation of the 4-ADFA Product. For the reaction of aniline with nitrobenzene by the action of the reaction system of a solution of trimethylammonio-acetate with potassium hydroxide a device was used, consisting of a reactor with a volume of 250 l, provided with a rapid agitator, a tempering jacket which was heated by warm water to regulate the temperature in the reactor, a nitrogen inlet under the surface of the reaction mixture, a condensator for condensation of vapours from the reactor, and a receiver for condensate collection which was used as a phase separator, and it was provided with an overflow for recycling the aniline phase with a content of nitrobenzene back to the reactor, while the separated aqueous phase of the condensate was permanently removed from the phase separator. The reactor was further provided with a thermometer and a pressure regulator. 19.1 l of distilled water, 12.8 kg of solid KOH, containing 86.5% of KOH, were inserted into an auxiliary vessel having the volume of 50 l, and after it had dissolved, 26.6 kg of betaine hydrate were added. After dissolving of all components the reaction system in the form of an aqueous solution was prepared to be used in the reaction. 111.8 kg (1.2 kmol) of aniline were inserted into the reactor, and 58.5 kg of the above given solution were added. The reactor was closed and was purged by nitrogen once, while the mixture was stirred. After termination of the reactor purging by nitrogen an absolute pressure of 20 kPa was set in the reactor, and the reactor content was gradually heated up to a temperature of 80° C. After reaching the temperature 21.1 kg of nitrobenzene (0.17 kmol) were started to be dosed into the reactor at such a rate that all nitrobenzene was fed within 1.5 h. The azeotrope aniline-water which was distilled off the reactor was collected in the receiver, where aqueous and aniline phase were separated. The aniline phase contained a certain amount of nitrobenzene and, therefore, it was periodically recycled to the condensation reactor during the whole experiment. After completing the dosing of nitrobenzene pressure in the reactor was gradually reduced to a value of 14 kPa, and the reaction mixture reacted at this pressure and at a temperature of 80° C. for 1.5 h. Then the pressure was gradually reduced to 8 kPa, and at this pressure the reaction mixture reacted for 1.5 h. Finally, pressure in the reactor was reduced to the value 4 kPa, and the reaction mixture was let to complete the reaction within 1.5 h. Finally it was cooled down to 40° C., approximately 15% of methanol were added, it was discharged from the reactor and weighed. An analysis of the reaction mixture has shown that 100% conversion of nitrobenzene took place with the following yield (in %) of individual reaction components (calculated in relation to the introduced nitrobenzene): 4-NODFA 77.0%; 4-NO2DFA 14.3%; 4-phenylazodiphenylamine 0.21%; azobenzene 9.6%; phenazine 1.3%. Note: Content of N-methylaniline was less than 0.05%, related to the introduced betaine. Reaction mixture from the condensation was diluted by methanol in such a way that its content in the diluted condensation mixture was 30% by weight, and it was hydrogenated under conditions, given in Example 19. A withdrawn sample of the reaction mixture was analyzed for the content of 4-ADFA. The overall yield of 4-ADFA, related to the starting content of 4-NODFA, 4-NO2DFA and 4-FADFA, was 99.2%. The yield of 4-ADFA in the hydrogenate, related to the nitrobenzene reacted, was 89.9%. After completing the hydrogenation the catalyst Raney Ni was filterred off, and it was washed by methanol and distilled water. The washing solutions were added to the hydrogenate. Methanol was distilled off the diluted hydrogenate at an absolute pressure of 35 kPa and at a temperature of 60 to 70°

References:

US6388136,2002,B1 Location in patent:Page column 13-15

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