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作 者:崔慧玲[1] 王丽红[1] 白官[1] 李笃信[1] 林培华[1]
出 处:《应用化工》2006年第4期295-297,共3页Applied Chemical Industry
摘 要:以咔唑为起始原料,经亚硝化和还原两步反应合成N-氨基咔唑。在亚硝化反应中,采用二甲基亚砜为溶剂,咔唑与亚硝酸钠反应的摩尔比为2.4:5.8,反应最佳温度为27-30℃,反应时间为2h,产率为86%。在还原反应中采用无水乙醇和冰醋酸的混和溶剂,两种溶剂的体积比为2:1,以锌粉为还原剂,反应温度为25~35℃,反应时间为2h,产率为81%。目的物及中间体经IR、^1H NMR及元素分析测试,证明其结构是正确的,同时对产物的荧光性质进行了初步研究。A new synthesis method of N-amino-carbazole was studied in this article. It was synthesized on the basis of carbazole by two steps reaction of nitrosation and reduction. The DMSO was used as solvent in nitrosation reaction,which the mole ratio of carbazole to NaNO2 was 2.4: 5.8, reacted for 2 h at 27- 30℃ ,the yield was 86%. Anhydrous alcohol and glacial acetic acid were used as component solvent, which the volume ratio was 2:1 ,zinc dust as reductant,reaction temperature was 25 -35℃ ,reaction time was 2 h,the yield was 81%. The structures of object compound and intermediate were identified by IR, ^1H NMR and elementary analysis. And their fluorescence characteristic were researched.
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