湖北大学学报(自然科学版)
湖北大學學報(自然科學版)
호북대학학보(자연과학판)
2013年
3期
358-360,380
,共4页
胡泉源%付方%张雄志%涂娇娇
鬍泉源%付方%張雄誌%塗嬌嬌
호천원%부방%장웅지%도교교
2-乙酰吡啶%碳酸二甲酯%4′-羟基-2 ,2′:6′,2″-三联吡啶%一锅法
2-乙酰吡啶%碳痠二甲酯%4′-羥基-2 ,2′:6′,2″-三聯吡啶%一鍋法
2-을선필정%탄산이갑지%4′-간기-2 ,2′:6′,2″-삼련필정%일과법
2-acetyl pyridine%dimethyl carbonate%4′-hydroxy-2,2′:6′,2″-terpyridine%one-pot synthesis
在无水乙醇中,以乙醇钠为碱、2-乙酰吡啶与碳酸二甲酯为原料合成1,3,5-三酮中间体,不经纯化,继续与氨水发生关环反应,一锅法合成了4′-羟基-2,2′:6′,2″-三联吡啶,收率50%。此方法文献少见报道,合成步骤简单,产品易于纯化,收率较高。对反应收率受反应溶剂、碱性条件、反应温度、反应时间的影响进行了讨论。
在無水乙醇中,以乙醇鈉為堿、2-乙酰吡啶與碳痠二甲酯為原料閤成1,3,5-三酮中間體,不經純化,繼續與氨水髮生關環反應,一鍋法閤成瞭4′-羥基-2,2′:6′,2″-三聯吡啶,收率50%。此方法文獻少見報道,閤成步驟簡單,產品易于純化,收率較高。對反應收率受反應溶劑、堿性條件、反應溫度、反應時間的影響進行瞭討論。
재무수을순중,이을순납위감、2-을선필정여탄산이갑지위원료합성1,3,5-삼동중간체,불경순화,계속여안수발생관배반응,일과법합성료4′-간기-2,2′:6′,2″-삼련필정,수솔50%。차방법문헌소견보도,합성보취간단,산품역우순화,수솔교고。대반응수솔수반응용제、감성조건、반응온도、반응시간적영향진행료토론。
4′-Hydroxy-2 ,2′:6′,2″-terpyridine was synthesized in one-pot reaction in yield of 50% . The intermediate 1 ,3 ,5-trione intermediate was synthesized from 2-acetyl pyridine and dimethyl carbonate in ethanol ,sodium ethoxide used as the base .The trione ,without any purification ,then reacted with ammnium solution immediately to accomplish a ring closure reaction . The synthetic method was easy to handle and purify with a hight yield ,and had never been reported before .The detail experimental conditions ,such as solvent ,base ,chemical reaction temperature and time ,were also discussed .