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5(6)-羧基罗丹明110的合成工艺
引用本文:高勇,杨晓航,游楚楚,欧阳翰,袁耀锋.5(6)-羧基罗丹明110的合成工艺[J].化工学报,2011,62(2):374-377.
作者姓名:高勇  杨晓航  游楚楚  欧阳翰  袁耀锋
作者单位:福州大学化学化工学院;陕西中医学院医学技术系;福建师范大学化学与材料学院
摘    要:研究了反应时间、升温方式、氮气保护等合成条件对5 (6)-羧基罗丹明110合成反应的影响,并利用基质辅助激光解吸电离飞行时间质谱对5 (6)-羧基罗丹明110的合成反应进行了检测。通过实验确定了较为适宜的合成条件:在氮气保护下80℃反应1 h,然后在30 min内匀速升温至180℃再反应6 h。在此条件下反应基本完全,磺化物较少,且可以通过重结晶除去。产率可达93%。

关 键 词:5(6)-羧基罗丹明110  基质辅助激光解吸电离飞行时间质谱  合成

Synthesis of 5(6)-carboxy-rhodamine 110
GAO Yong,YANG Xiaohang,YOU Chuchu,OUYANG Han,YUAN Yaofeng.Synthesis of 5(6)-carboxy-rhodamine 110[J].Journal of Chemical Industry and Engineering(China),2011,62(2):374-377.
Authors:GAO Yong  YANG Xiaohang  YOU Chuchu  OUYANG Han  YUAN Yaofeng
Abstract:The influence of some factors on synthesis of 5(6)-carboxy-rhodamine 110 was investigated, such as reaction time, heating mode, and nitrogen atmosphere.MALDI-TOF mass spectrometry was used for monitoring the synthesis reaction.The optimized reaction conditions are as follows.Under the protection of nitrogen, after reaction at 80℃ for 1 h the temperature is raised to 180℃ at a constant rate within 30 min.Then the reaction is maintained at the temperature for 6 h.Under the conditions the reaction is nearly completed.A little of sulfonated derivatives formed in the reaction can be purified by recrystallization.The yield is 93%.
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