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1h,然后在30min内匀速升温至180℃再反应6h。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%。
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%.
出处
《化工学报》
EI
CAS
CSCD
北大核心
2011年第2期374-377,共4页
CIESC Journal
基金
福建省自然科学基金项目(2009J05023)~~