以邻香草醛和4,4′-二氨基二苯醚为原料,合成双邻香草醛希夫碱。通过单因素实验讨论了不同溶剂、反应时间、反应温度和物料物质的量之比对希夫碱产率的影响,并采用IR、1H 和13C核磁、元素分析等手段对产物希夫碱结构进行了表征。希夫碱合成的适宜工艺条件为:溶剂为四氢呋喃,反应温度35 ℃,反应时间1 h,邻香草醛与4,4′-二氨基二苯醚的物质的量之比为2〖DK〗∶1,在此条件下希夫碱产率达到697 %。
Abstract
Bis(Ovanillin) benzoilimine Schiff base was syntheticed with ovanillin and 4,4′diaminodiphenyl ether as raw materials. Effects of solvents,reaction temperature and time, and molar ratio on the yield of Schiff base were examined. The structure of the schiff base was characterized with IR,1H NMR,13C NMR,and elemental analysis. The optimum synthesis condition was shown as follows: molar ratio of ovanillin to 4,4′-diaminodiphenyl ether 2〖DK〗∶1; tetrahydrofuran as the solvent; reaction temperature 35 ℃, and reaction time 1 h. The yield of Schiff base was reached 697 %.
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基金
收稿日期:2010-11-04修回日期:2011-04-23基金项目:广西林产化学品开发与应用重点实验室开放基金项目(GXFC08-08)作者简介:蔡奔(1985—),硕士生。*罗金岳(通信作者),教授。Email: luojinyue@njfu.com.cn