CAJ | 학술논문

针对荧光染料中间体3，6-二氯-苯三甲酸酐的产率偏低、重现性差的问题，对其合成方法进行改进。以2，5-二氯-对二甲苯为原料，选择无水乙醚为反应介质，经酰化、氧化，再直接脱水得到荧光染料中间体3，6-二氯-苯三甲酸酐。产物及中间体结构通过1 HNMR、MS、HPLC和元素分析表征。实验结果表明1-（2，5-二氯-3，6-二甲基苯基）乙酮合成中的最佳反应条件：反应时间为26 h，2，5-二氯-对二甲苯与乙酰氯最佳配比为1∶3，改进后反应三步总产率比相关文献报道值高出15％。
침대형광염료중간체3，6-이록-분삼갑산항적산솔편저、중현성차적문제，대기합성방법진행개진。이2，5-이록-대이갑분위원료，선택무수을미위반응개질，경선화、양화，재직접탈수득도형광염료중간체3，6-이록-분삼갑산항。산물급중간체결구통과1 HNMR、MS、HPLC화원소분석표정。실험결과표명1-（2，5-이록-3，6-이갑기분기）을동합성중적최가반응조건：반응시간위26 h，2，5-이록-대이갑분여을선록최가배비위1∶3，개진후반응삼보총산솔비상관문헌보도치고출15％。
In order to solve the low yield and poor reproducibility of 3,6-dichloro-trimellitic anhydride, its synthesis method is improved.The compound 3,6-dichloro-trimellitic anhydride is obtained from the starting material 2,5-dichloro-p-xylene in anhydrous ether via acylation,oxidation and dehydration.The structures of the target compound and intermediates are determined by 1 HNMR,MS and HPLC,and characterized by elemental analysis.The results show that the optimum synthetic reaction conditions of 1-(2,5-dichloro-3,6-dimethylphenyl)ethanone are as following:26 h of the reaction time,mass ratio of 2,5-dichloro-p-xylene and acetyl chloride of 1 ∶3.The yield of the addition reaction is increased 15%because the synthesis method is improved.