Zhang Fe
2014
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Journal
Fine chemicals
Abstract
4,5-Dibromophthalic acid was an intermediate for the synthesis of carboxyl substituted phthalocyanine compounds. In the presence of the solvent methylene chloride,4,5-dibromo-o-xylene was synthesized from o-xylene and bromide through electrophilic substitution reaction. Then,it went through the oxidation with potassium permanganate to give 4,5-dibromophthalic acid. By studying the process conditions,we got the optimal reaction conditions of 4,5-dibromo-o-xylene as follows: Br 2 volume concentration 40%,o-xylene volume concentration 40%,Br 2 ∶I 2 ∶o-xylene( 3. 0∶0. 15∶1. 0,molar ratio). By amplifying the experimental conditions by 10 times,we got the yield of 79. 0%. And the optimal reaction conditions of 4,5-dibromophthalic acid were: potassium permanganate,phase transfer catalyst and 4,5-dibromo-o-xylene whose molar ratio were 6. 0 ∶ 0. 04 ∶ 1. 0,reaction time 10 h, temperature 100 ℃. By amplifying the experimental conditions by 10 times,we got the yield of 85. 5%, which was higher than the reported yields of 71. 0% and 77. 0%.