Controlled feed process for making 3, 5-diaminobenzotrifluoride

Details Controlled feed process for making 3, 5-diaminobenzotrifluoride Controlled feed process for making 3, 5-diaminobenzotrifluoride

1992-08-17

1997-05-13

Kumar, Shailendra

Organic compounds -- part of the class 532-570 series

Organic compounds

Amino nitrogen containing

564415, 564416, 564422, 564423, C07C20932

Patent

active

056294492

ABSTRACT:
Disclosed is a method of making 3,5-diaminobenzotrifluoride from 4-chloro-3,5-dinitrobenzotrifluoride. A solution of 4-chloro-3,5-dinitrobenzotrifluoride in an alcohol is prepared. Separately, a slurry is prepared of a palladium catalyst on a suitable substrate, at least one equivalent of magnesium oxide per equivalent of 4-chloro-3,5-dinitrobenzotrifluoride, sufficient hydrogen-donating reducing agent to reduce the 4-chloro-3,5-dinitrobenzotrifluoride to 3,5-diaminobenzotrifluoride, and an amount of alcohol sufficient to make the slurry stirrable. The solution is added to the slurry with stirring at a rate that does not exceed the reaction rate of the 4-chloro-3,5-dinitrobenzotrifluoride so that no unreacted 4-chloro-3,5-dinitrobenzotrifluoride accumulates in the slurry. The reaction mixture is heated at about 75.degree. to about 100.degree. C.

REFERENCES:
patent: 3073865 (1963-01-01), Spiegler
patent: 5144076 (1992-09-01), Krishnamurti et al.
J. Chem. Soc. Perkin Trans. II 1986 pp. 187-192, 1986.

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