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作 者:廖波[1] 刘建军[1] 李保山[1] 左胜利[1]
出 处:《合成化学》2016年第7期635-638,共4页Chinese Journal of Synthetic Chemistry
摘 要:以1,6-亚甲基桥[10]轮烯-3,4-二甲酸酐为原料,与羟胺基盐酸盐经酰化和脱水反应制得N-羟基-1,6-亚甲基桥[10]轮烯-3,4-酰亚胺(2);构建了2/乙酸钴催化体系,以氧分子为氧源,乙腈为溶剂,在1 MPa氧气压力下于120℃反应20 h,氧化3-甲基吡啶制备烟酸,产率70%,其结构经-1H NMR和IR确证。Synthesis of N-hydroxy-1,6-methano [ 10 ] annulene-3,4-dicarboximide ( 2 ) was accom- plished by acylation and dehydration of hydroxylamine hydrochloride using 1,6-methano [ 10 ] annulene- 3,4-dicarboxylic anhydride as starting material. 2/Cobalt(II) acetate catalytic system was built by u- sing oxygen molecule as oxygen source and acetonitrile as solvent. The yield of nicotinic acid was 70% after oxidative reaction of β-picoline at 120 ℃ for 20 h with 1 MPa of oxygen pressure. The structure was confirmed by l H NMR and IR.
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