武汉轻工大学学报
武漢輕工大學學報
무한경공대학학보
Journal of Wuhan Polytechnic University
2014年
3期
42-45
,共4页
陈莎娜%陈新%周有骏%周浩
陳莎娜%陳新%週有駿%週浩
진사나%진신%주유준%주호
四氢喹喔啉类化合物%合成工艺%正交实验
四氫喹喔啉類化閤物%閤成工藝%正交實驗
사경규악람류화합물%합성공예%정교실험
1,2,3,4-tetrahydroquinoxaline derivatives%synthesis%orthogonal experiment
优化N-取代苯基四氢喹喔啉类化合物的合成工艺,考察各实验条件对关键中间体2-苯基-1,2-二氢喹喔啉合成的影响。设计最新合成路线;平行实验比较碳酸钠和乙酸钠对环合反应的影响,并对实验结果进行总体分析;对碳酸钠催化环合反应进行正交实验设计,考察反应温度和溶剂对收率的影响。结果显示:碳酸钠催化环合反应的收率较高,且易于处理;正交实验结果表明,以碳酸钠为催化剂,甲醇为溶剂进行室温反应,为环合反应的最优实验方案,收率达91.43%;新合成路线的总收率达67.64%。新合成方法步骤简单,条件温和,收率较高,适用于大量制备。
優化N-取代苯基四氫喹喔啉類化閤物的閤成工藝,攷察各實驗條件對關鍵中間體2-苯基-1,2-二氫喹喔啉閤成的影響。設計最新閤成路線;平行實驗比較碳痠鈉和乙痠鈉對環閤反應的影響,併對實驗結果進行總體分析;對碳痠鈉催化環閤反應進行正交實驗設計,攷察反應溫度和溶劑對收率的影響。結果顯示:碳痠鈉催化環閤反應的收率較高,且易于處理;正交實驗結果錶明,以碳痠鈉為催化劑,甲醇為溶劑進行室溫反應,為環閤反應的最優實驗方案,收率達91.43%;新閤成路線的總收率達67.64%。新閤成方法步驟簡單,條件溫和,收率較高,適用于大量製備。
우화N-취대분기사경규악람류화합물적합성공예,고찰각실험조건대관건중간체2-분기-1,2-이경규악람합성적영향。설계최신합성로선;평행실험비교탄산납화을산납대배합반응적영향,병대실험결과진행총체분석;대탄산납최화배합반응진행정교실험설계,고찰반응온도화용제대수솔적영향。결과현시:탄산납최화배합반응적수솔교고,차역우처리;정교실험결과표명,이탄산납위최화제,갑순위용제진행실온반응,위배합반응적최우실험방안,수솔체91.43%;신합성로선적총수솔체67.64%。신합성방법보취간단,조건온화,수솔교고,괄용우대량제비。
To optimize Synthesis of N-substituted 3-benzyl-1,2,3,4-Tetrahydroquinoxaline derivatives and investi-gate the influence of experiment condition in the synthesis of key intermediate 2-benzyl-1,2-dihydroquinoxaline . Methods:A novel synthesis methods was designed;a parallel test was carried out to compare the catalytic activity of sodium carbonate and sodium acetate in cyclization reaction , including the total analysis of experimental result;And orthogonal experimental design was applied and the influence of temperature and solvent on the yield were in -vestigated .Results:The yield of the Sodium carbonate was higher than that of sodium acetate with easy effluent dis-posal, Orthogonal test confirms that Sodium carbonate used as catalyst , methanol as solvent in r .t.are the optimal experiment scheme and the yield is 91 .43%.The total yield is 67 .64%.Conclusion:the synthesized methods are much more available for large-scale preparation with easier procedure and higher yield .