张明政,李然,黄丹.化学通报,2014,77(12):1201.
1,2-环氧丙醚基芳香酮紫外线吸收剂的微波合成和表征
Microwave synthesis and characterization of 1,2-epoxy propyl ether aromatic ketone UV absorbents
投稿时间:2014-06-20  修订日期:2014-08-15
DOI:
中文关键词:  微波合成  反应性紫外线吸收剂  2,4-二羟基二苯甲酮  4-羟基苯乙酮  环氧氯丙烷
英文关键词:microwave synthesis  UV absorbers with reactive groups  2,4-dihydroxybenzophenone  4-hydroxyacetophenone  epichlorohydrin
基金项目:苏州大学有机合成江苏省重点实验室开放课题资助项目
作者单位E-mail
张明政 江南大学生态纺织教育部重点实验室 江苏省无锡市 214122 375913832@qq.com 
李然 江南大学生态纺织教育部重点实验室 江苏省无锡市 214122  
黄丹* 江南大学生态纺织教育部重点实验室 江苏省无锡市 214122 huangdan6@163.com 
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中文摘要:
      以2,4-二羟基二苯甲酮(UV-O)、4-羟基苯乙酮(HAP)为原料分别和环氧氯丙烷反应,经微波辐照合成了两种反应性紫外线吸收剂2-羟基-4-缩水甘油醚基二苯甲酮(HEPBP)和4-缩水甘油醚基苯乙酮(EPAP)。结构采用红外光谱、核磁和质谱表征。最佳的合成条件为:n(羟基芳香酮):n(环氧氯丙烷)=1:3,微波功率400W,于90℃反应15min,收率分别是52.6%和58.3%。与常规合成方法比较,微波合成法能降低反应温度、大大地缩短反应时间。产物中环氧丙烷基团的引入能提高芳香酮类紫外线吸收剂的紫外吸收性能。
英文摘要:
      Two reactive UV absorbers, 2-hydroxy-4(2,3-epoxypropoxy)-benzophenone and 4(2,3-epoxypropoxy)- acetophenone were synthesized by reaction of hydroxylated aromatic ketone (2,4-dihydroxybenzophenone and 4-acetophenone) and epichlorohydrin under microwave radiation and characterized by IR, NMR, MS and UV–vis. The optimal reaction conditions were as follows: molar ratio ofhydroxylated aromatic ketone and epichlorohydrin was 1:3, microwave power was 400W in sodium hydroxide solution at 90℃ for 15min. The yield was 52.6% and 58.3% under the conditions. Comparing with the conventional synthesis process, microwave synthesis can reduce the reaction temperature, greatly shorten the reaction time. The ultraviolet absorption properties of aromatic ketone ultraviolet absorbers were improved significantly as epoxy propane groups introduced.
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