Hydrochloric Acid → 2-Chloro-4-nitroaniline

Participants

Reaction Steps

A process for the preparation of substantially pure 2,6-dichloro-4nitroaniline by chlorinatin of 4-nitroaniline with chloring bleaching liquor in water using acids, which comprises chlorinating 1 mole of 4-nitroaniline in 3-6 mole of hydrochloric acid (HCl) or nitric acid (HNO3) in the form of a dilute, aqueous acid in the presence of a dispersing agent which is stable under the reaction conditions, the chlorination initially being carried out at 5° to 10° C. and then at 15°-20° C. and, finally, after 90-95% of the 2-chloro-4-nitroaniline intermediately formed has been converted into 2,6-dichloro-4-nitroaniline, the temperature of the aqueous suspension being increased from 15°-20° C. to 70° C., without further addition of chlorine bleaching liquor, and then by post-chlorinating, by renewed addition of chlorine bleaching liquor, at temperatures between 20 ° and 70° C., bringing the pH of the aqueous sispension to 9.0 and filtering off the 2,6-dichloro-4-nitroaniline formed and washing it with dilute mineral acid to provide 2,6-dichloro-4-nitroaniline of a purity of 96% or above, and a melting point of 187°-191° C. and in a yield of 80% or above.

Provenance & Evidence