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EXP10 Synthesis of p Bromoaniline | Amine | Molecules
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Synthesis of p-bromoaniline lab - Gershom scholem …
SUBSTANCE: invention relates to a solution used in synthesis of 4-aminodiphenylamine. Method involves the condensation reaction of nitrobenzene with aniline followed by catalytic hydrogenation of prepared mixture of 4-nitroso- and 4-nitrodiphenylamine tetramethylammonium salts containing aniline, potassium chloride and water. The solution contains additionally aniline tetramethylammonium salt of the formula: C6H5NHM wherein M represents tetramethylammonium cation (CH3)4N+ in the following ratio of components, wt.-%: C6H5NHM, 18.2-22.6; aniline, 52.0-64.7; water, 11.0-28.4; KCl, 1.4-1.7. Method for preparing the claimed solution used for synthesis of 4-aminodiphenylamine involves dissolving tetramethylammonium chloride in water, addition of equivalent amount of potassium hydroxide, removal of potassium chloride excess by filtration and addition of aniline to filtrate. Method for preparing 4-aminodiphenylamine by using the claimed solution involves the condensation reaction of aniline tetramethylammonium salt of the formula C6H5NHM wherein M represents tetramethylammonium cation (CH3)4N+ with nitrobenzene in aniline medium and the following distilling off water to obtain a mixture of 4-nitroso- and 4-nitrodiphenylamine tetramethylammonium salts. By termination of the condensation reaction tetramethylammonium hydroxide is removed and the remaining mixture of 4-nitroso- and 4-nitrodiphenylamine is hydrogenated catalytically to 4-aminodiphenylamine in medium consisting of aniline, toluene and water. Using the claimed solution provides increasing the yield of 4-aminodiphenylamine, and to simplify and reduce cost of the process.
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