4-溴邻苯二甲酸二异辛酯的合成  

Synthesis of Di-iso-octyl 4-Bromophthalic Anhydride

作　　者：王智方[1] 孙树娟[1] 李效军[1] 雒佳丽[1] 

机构地区：[1]河北工业大学化工学院,天津300130

出　　处：《安徽农业科学》2009年第17期7814-7815,共2页Journal of Anhui Agricultural Sciences

摘　　要：[目的]考察4-溴邻苯二甲酸二异辛酯的合成工艺条件。[方法]以苯酐、溴素及异辛醇为主要起始原料，经溴化反应得到4-溴邻苯二甲酸，再经酯化反应合成4-溴邻苯二甲酸二异辛酯。通过考察原料的摩尔比、反应时间及催化剂用量等关键因素对试验结果的影响，研究合成的优化条件。[结果]酯化反应中较优的合成条件是：催化剂浓硫酸的用量为总原料质量的4％，4-溴邻苯二甲酸与异辛醇的摩尔比为1：5，反应时间为5h，以苯酐计产品的综合收率为87．13％，试验所得产品经气相色谱分析含量在昕％以上，产品结构经^1H—NMR分析确定与目标产物相符。[结论]产物的表征为，4-溴邻苯二甲酸，^1H—NMR（D2O）：8．52（s，1H）；8．23（s，1H）；7．98（s，1H）；4-溴邻苯二甲酸二异辛酯，^1H—NMR（CDCl3）：8．25（s，1H）；7．97（s，1H）；7．73（s，1H）；4．20—4．28（m，4H）；2．05～2．12（m，2H）；1．25～1．33（m，16H）：0．94～0．99（12H）。[Objective] The aim was to investigate the synthesis process conditions of di-iso-nctyl 4-bromophthalate. [Method] With phthalie anhydride, bromine and isonctyl alcohol as main starting materials the 4-bromophthalic anhydride was obtained by means of bromination reaction and then di-iso-octyl 4- bromophthalate was synthesized after esterification. The optimum conditions for synthesis were studied by investigating the effects of key factors of molar ratio of raw materials, reaction time and catalyst amount etc. on experiment result. [Result] The better synthesis conditions in estefification were： the dosage of catalyst concentrated sulfuric acid was 4% of total raw material mass, the molar ratio of 4-bromophthalic anhydride and isonctyl alcohol was 1：5, reaction time 5h, the comprehensive yield counting with phthalic anhydride was 87.13%, the content of product acquired from test was over 97% after gas chromatography analysis, and the product structure was conformed to target product through ^H-NMR analysis arid determination. [Conclusion] The characterization of the product was 4-bromophthalic anhydride,^1H-NMR（D2O）： 8.52（s, 1H）; 8.23（s, 1H）; 7.98（s, 1H）; di-iso-octyl 4-bromophthalate,^1H-NMR（CDCl3）： 8.25（s, 1H）; 7.97（s,1H）;7.73（s,1H）; 4.20-4.28（m,4H）; 2.05-2.12（m,2H）; 1.25-1.33（m,16H）; 0.94-0.99（12H）.

关 键 词：邻苯二甲酸酐 溴化反应 酯化反应 

分 类 号：O625.5[理学—有机化学]