Process for the preparation of 1,3,5-triaminobenzene and its hydrolysis to high purity phloroglucinol

摘要

Preparing 1,3,5-triamino benzene comprises amination of a halobenzene (I) in the presence of ammonia and a catalyst selected from copper salts, cuprous and cupric oxides, and their mixtures, at a temperature of 150 - 250degreesC and a pressure above 35 bars. Preparing 1,3,5-triamino benzene comprises amination of a halobenzene of formula (I) in the presence of ammonia and a catalyst selected from copper salts, cuprous and cupric oxides, and their mixtures, at a temperature of 150 - 250degreesC and a pressure above 35 bars. A = halogen or NH2; X1, X2 = halogen. Independent claims are included for: (a) preparing phloroglucinol from 1,3,5-triamino benzene prepared as above, comprising hydrolysis in the presence of HCl or H2SO4 above 90degreesC for 6 - 24 hours, optionally filtering the reaction mixture at ambient temperature, and extracting the phloroglucinol formed using diethyl ether or an ester, especially ethyl benzoate, ethyl acetate, isopropyl acetate, or n-butyl acetate; (b) phloroglucinol prepared by this process containing less than 0.5 % impurities; and (c) the medicinal use of phloroglucinol prepared as in (b).