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兴发pt登录学报,2019,36(9):18-21https://doi.org/10.16039/j.cnki.cn22-1249.2019.09.005
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2-(4-吡啶基)-4,5-二氢恶唑的催化合成
李鑫,邱俊
兴发pt登录 化学与制药工程学院
Catalytic Synthesis of 2-(pyridin-4-yl)-4,5-dihydrooxazole
LI Xin, QIU Jun
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摘要

采用浸渍法制备了分子筛负载氧氯化锆催化剂ZrOCl2·8H2O/H-BEA、ZrOCl2·8H2O/H-USY、ZrOCl2·8H2O/H-ZSM-5和ZrOCl2·8H2O/H-MCM-41,并在无溶剂条件下考察了它们催化4-氰基吡啶与乙醇胺缩合反应合成2-(4-吡啶基)-4,5-二氢恶唑的性能。结果表明,这些催化剂都表现出较高的催化活性,活性主要源于ZrOCl2·8H2O同时也受载体比表面积和酸性位数量影响,其中ZrOCl2·8H2OH-MCM-41的活性最高。在优化的工艺条件下,10% ZrOCl2·8H2O/H-MCM-41催化剂上,催化剂用量为反应原料质量的10%、4-氰基吡啶与乙醇胺摩尔比为1:2、温度为110 ℃下反应为180 min, 2-(4-吡啶基)-4,5-二氢恶唑的产率达到98.4%。

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李鑫
邱俊
关键词:4-氰基吡啶乙醇胺分子筛催化ZrOCl2·8H2O2-(4-吡啶基)-4,5-二氢恶唑
Abstract:

In this paper, the catalysts of zirconium oxychloride on molecular sieve were prepared by immersion, and which was employed to catalyze the condensation reaction of 4-cyanopyridine and ethanol amine for synthesizing the pharmaceutical intermediates of 2-(pyridin-4-yl)-4,5-dihydrooxazole under solvent-free conditions. The resultants were identified by gas chromatography - mass spectrometry and the contents were determined by gas chromatography. The results indicated that, These catalysts all exhibit high catalytic activity. The activity is mainly derived from ZrOCl2·8H2O. It is also affected by the specific surface area of the carrier and the number of acidic sites. ZZrOCl2·8H2O/H-MCM-41 has the highest activity. By single factor multi-levels experiments, the optimal technology for the synthesis of 2-(pyridin-4-yl)-4,5-dihydrooxazole was obtained. The optimal conditions were as follow: the molar rate of 4-cyanopyridine to ethanol amine was 1:2, 10% ZrOCl2·8H2O/H-MCM-41 was used as catalyst, catalyst dosage was 10% mass of reactants, reacted at 110 ℃ for 3 h. Under the optimum technology, the conversion of 3-cyanopyridine was up to 98.4%.

Key words:4-cyanopyridineethanolaminemolecular sievecatalysisZrOCl2·8H2O2-(pyridin-4-yl)-4,5-dihydrooxazole
出版日期:2019-09-25发布日期:2019-09-25整期出版日期:2019-09-25
ZTFLH: TQ203.2
引用本文:
李鑫, 邱俊. 2-(4-吡啶基)-4,5-二氢恶唑的催化合成 [J]. 兴发pt登录学报, 2019, 36(9): 18-21.
LI Xin, QIU Jun. Catalytic Synthesis of 2-(pyridin-4-yl)-4,5-dihydrooxazole. Journal of Jilin Institute of Chemical Technology, 2019, 36(9): 18-21.
链接本文:
http://xuebao.jlict.edu.cn/CN/10.16039/j.cnki.cn22-1249.2019.09.005http://xuebao.jlict.edu.cn/CN/Y2019/V36/I9/18
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