辽东学院学报(自然科学版)
遼東學院學報(自然科學版)
료동학원학보(자연과학판)
JOURNAL OF LIAODONG UNIVERSITY(NATURAL SCIENCES)
2013年
4期
229-232
,共4页
二氯烟酰氯%酰化反应%含氮杂环化合物%合成
二氯煙酰氯%酰化反應%含氮雜環化閤物%閤成
이록연선록%선화반응%함담잡배화합물%합성
2-chloronicotinyl chloride%acidylation reaction%heterocyclic nitrogen compound%synthesis
以2-氯烟酰氯和含氮的六元杂环化合物为起始原料,经酰化反应合成了6个2-氯吡啶-3-碳酰-含氮杂化化合物,收率达70%以上。同时考察了反应原料的物质的量之比和溶剂乙酸乙酯和水的体积之比对目标产物收率的影响,得到的最佳反应条件: n(二氯烟酰氯)∶n(含氮杂环化合物)=1∶1,V(乙酸乙酯)∶V(水)=1∶1。产物经核磁、质谱、元素分析等进行了表征。
以2-氯煙酰氯和含氮的六元雜環化閤物為起始原料,經酰化反應閤成瞭6箇2-氯吡啶-3-碳酰-含氮雜化化閤物,收率達70%以上。同時攷察瞭反應原料的物質的量之比和溶劑乙痠乙酯和水的體積之比對目標產物收率的影響,得到的最佳反應條件: n(二氯煙酰氯)∶n(含氮雜環化閤物)=1∶1,V(乙痠乙酯)∶V(水)=1∶1。產物經覈磁、質譜、元素分析等進行瞭錶徵。
이2-록연선록화함담적륙원잡배화합물위기시원료,경선화반응합성료6개2-록필정-3-탄선-함담잡화화합물,수솔체70%이상。동시고찰료반응원료적물질적량지비화용제을산을지화수적체적지비대목표산물수솔적영향,득도적최가반응조건: n(이록연선록)∶n(함담잡배화합물)=1∶1,V(을산을지)∶V(수)=1∶1。산물경핵자、질보、원소분석등진행료표정。
Six ( 2-chloro-pyridin-3-carbonyl ) -heterocyclic nitrogen compounds with a yield of over 70%were prepared from corresponding heterocyclic nitrogen compounds , which was reacted with 2-chloronicoti-noyl chloride .The effect of the proportion of raw materials as well as that of acetic ether and water on target product was studied .It was found that the best yield was obtained when the mole ratio of 2-chloronicotinoyl chloride to the starting heterocyclic nitrogen compounds was 1∶1 and the volume ratio of acetic acid ethyl ester to water was 1∶1 . The structures of all products were characterized by melting point , Mass, 1 HNMR and elemental analysis .