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机构地区:[1]浙江工业大学化学工程与材料学院,浙江杭州310014
出 处:《合成化学》2008年第2期210-212,216,共4页Chinese Journal of Synthetic Chemistry
摘 要:以间二乙氨基苯酚(1)和邻苯二甲酸酐(2)为原料制得2-羧基-4′-二乙氨基-2′-羟基二苯甲酮(3);在浓硫酸作用下,3与2-甲基-5-对甲氧基苯基-1,3,4-噁二唑(4)反应合成了一种新型的荧烷染料——2-(5-甲基-1,3,4-噁二唑-2-基)-6-二乙氨基荧烷,其结构经1H NMR,IR和元素分析表征。合成3的较适宜条件为:132mmol,n(1)∶n(2)=1.0∶1.2,36%NaOH 60 mL,反应时间10 h,分解时间6 h,收率71.8%,纯度83.4%(HPLC)。A novel fluorane dye, 2-( 5-methyl-1,3,4-oxadiazole-2-yl)-6-diethylaminofluoran, was synthesized by the reaction of 2-methyl-5- (p-methoxyphenyl) -1,3,4-oxadiazole ( 4 ) and 2-carboxyl- 4'-diethylamino-2'-hydroxy benzophenone ( 3 ) which was prepared from p-diethylamino phenol ( 1 ) and phthalic anhydride(2). The structures were confirmed by UV, ^1H NMR, IR and elemental analysis. The appropriate reaction conditions of synthesizing 3 in yield of 71.8% ( purity 83.4 by HPLC) were as follows: 1 was 32 mmol; n(1) :n(2) was 1.0 : 1.2; 36% NaOH was 60 mL; reaction time and decomposition time was 10 h and 6 h, respectively.
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