含联吡啶单元大环配体的合成

含联吡啶单元大环配体的合成 Syntheses of Macrocyclic Ligand Containing Bipyridine Subunit 何永炳 HE Yong\|bing 1 first-author 肖元晶 XIAO Yuan\|jing 1 孟令芝 MENG Ling\|zhi 1 武汉大学化学与环境科学学院,武汉,430072 武汉大学化学与环境科学学院,武汉,430072 College of Chemistry and Environment Science, Wuhan University, Wuhan 430072, China) \ College of Chemistry and Environment Science, Wuhan University, Wuhan 430072, China) \ 6,6′-二羟甲基-2,2′-联吡啶（1）经与3,4-二氢吡喃（DHP）反应得到6-羟甲基-6′-四氢吡喃（THP）氧甲基-2,2′-联吡啶（2）;化合物（2）经甲磺酰化和碘化反应得到6-碘甲基-6′-四氢吡喃氧甲基-2,2′-联吡啶（5）;（2）和（5）经缩合、醇解反应得到双（6′-羟甲基-2,2′-联吡啶-6-甲基）醚（7）;（7）与6,6′-二溴甲基-2,2′-联吡啶反应得到大环配体（8）. 对中间体（2）的合成条件进行了探讨. 所有中间体和大环配体均经元素分析、1 H NMR、MS等证实了它们的结构和组成. Hydroxymethyl 6′ tetrahydropyranyloxymethy1 2,2′ bipyridine（2） was synthesized by the reaction of 6.6′ dihydroxymethyl 2,2′ bipyridine（1） with 3,4 dihydropyran. 6 Tetrahydropyranyloxymethyl 6′ iodomethyl 2,2′ bipyridine（5） was obtained by reactions of mesylate and iodinating of compound（2）. Bis （6′ hydroxymethyl 2,2′ bipyridine 6 methyl） ether（7） was synthesized by the reaction of coupling of compound（2） with（5） and alcoholizing. Macrocyclic ligand（8） was obtained by treating compound（7） and 6,6′ dibromomethyl 2,2′ bipyridine. The synthetic conditions of the intermediate（2） was studied. All intermediates and macrocyclic ligand were identified by elemental analysis, 1H NMR and MS.\; 氮杂冠醚 联吡啶衍生物 合成 azacrown ether bipyridine derivative synthesis Q-33 1999-06-01 2021-04-01 6