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作 者:朱万仁[1] 丁树红[1] 陈光全[1] 李家贵[1] 张锡珍[1] 王艳丽[1]
机构地区:[1]玉林师范学院化学与生物系,广西玉林537000
出 处:《化学世界》2009年第9期553-556,共4页Chemical World
基 金:广西教育厅科研项目资助课题(桂教科研[2004]22号)
摘 要:报道以水杨醛、1,2-二氯乙烷为原料,合成中间体2,2'-双(1,2-二氧代乙基)苯甲醛,然后中间体再与邻氨基时甲苯酚合成开链冠醚的双水杨基亚胺新型席夫碱,并探讨了合成中间体的最佳合成条件,在水杨醛与1,2-二氯己烷物质的量之比为2.5:1时、溶液的pH为8、反应温度为70~80℃、反应达13h的产率达到48.0%;通常产物的合成PH值控制在8,物料比为1:2.4,反应12h,反应温度80。C,可以得到较高的产率78.5%。产物用元素分析、紫外光谐、红外光谱(KBr压片)、^1H NMR和^13C NMR进行了表征。Novel Schiff base of disalicyl imine of open chain crown ether was synthesized by the condensation of the intermediate, 2,2'-bi 1,2-bioxyethyl benzaldehyde and o-amino-p-methyl-phenol. The favorable conditions of preparing the intermediate were found, i.e. pH of reacting solution was 8, the reacting time was about 13 h, the reacting temperature was 70-80 ℃ and the mole ratio of salicylaldehyde to 1,2-dichroloethane was 2.5 to 1. The intermediate yield was 48.0 %. The conditions of synthesizing the Schiff base were that the pH of reacting solution was 8, the reacting time was about 12 h, the reacting temperature was 80℃ and that the mole ratio of o-amino-p-methyl-phenol to the intermediate was 2.4 to 1. The yield was 78.5%. The novel Schiff base was characterized by elemental, UV, IR, ^1H NMR and ^13 C NMR analyses.
关 键 词:2 2'-双(1 2-二氧代乙基)苯甲醛 双水杨基亚胺 合成
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