N-羟基-1,6-亚甲基桥[10]轮烯-3,4-酰亚胺/乙酸钴液相催化氧化3-甲基吡啶制备烟酸

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 Nicotinic Acid by Liquid-phase Oxidation ofβ-Picoline Catalyzed by N-hydroxyl-1,6-methano[10] annulene-3,4-dicarboximide/Cobalt(II) Acetate

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-methano10]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 1 H NMR and IR.