反应详情

温度

15 °C

4.00 g (0.0221 mol) trimellitic acid anhydride was dissolved in 60 ml 98% methane-sulfonic acid and 20 ml 98% sulfuric acid during 1 hour at 40° C. and was then cooled to 15° C. 4.99 g (0.125 mol) 85% hydrogen peroxide was added by drops during 15 minutes. After 2 hours at 30° C. the mixture was cooled and gently poured into 800 ml ice-cold (0°-10° C.) ethyl acetate under agitation, whereupon 200 ml saturated (NH4)2SO4 solution was added. After 2 hours vigorous agitation the ethyl acetate phase was separated and dried over Na2SO4. The ethyl acetate was evaporated until a viscous yellow-white oil remained. Diperoxy trimellitic acid crystallized in petroleum-ether/diethylether and was dried until constant weight. Titration on active oxygen showed a yield of 70.7%.

1. temperatureAfter 2 hours at 30° C. the mixture was cooled
2. additionwas added
3. customAfter 2 hours vigorous agitation the ethyl acetate phase was separated
4. dry with materialdried over Na2SO4
5. customThe ethyl acetate was evaporated until a viscous yellow-white oil
6. customDiperoxy trimellitic acid crystallized in petroleum-ether/diethylether
7. customwas dried until constant weight