Process for the preparation of n,n-dimethyl-n-(2-...

Details Process for the preparation of n,n-dimethyl-n-(2-... Process for the preparation of n,n-dimethyl-n-(2-...

C - Chemistry, Metallurgy

07

C

260/152

C07C 41/22 (2006.01) C07C 17/093 (2006.01)

Patent

CA 1145745

ABSTRACT A process for the preparation of N,N-dimethyl- N'-(2-bromo-4-methyl-phenyl)-triazene of the formula Image comprising (a) reacting N-acetyl-p-toluidine of the formula Image with bromine at a temperature between about 0 and 100°C, to give the intermediate product of the formula Image (b) reacting the intermediate product with hydrochloric acid by either i) adding a dilute solution of aqueous hydrochloric acid to the intermediate product in its reaction solution and heating the mixture to a temperature between about 50 and 120°C, or ii) precipitating the intermediate product from its reaction solution by mixing with water and filtering off, and without purification or drying heating the precipitate with dilute aqueous hydrochloric acid to a temperature between about 50 and 120°C, thereby to form a solution of 2-bromo-4-methylaniline hydrochloride, (c) reacting the resulting aqueous solution with an alkali metal nitrite at a temperature between about -20 and +30°C, and (d) reacting the product with dimethylamine at a temperature between about 0 and 50°C.

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