Facile synthesis of furfuryl ethyl ether in high yield via the reductive etherification of furfural in ethanol over Pd/C under mild conditions
Facile synthesis of furfuryl ethyl ether in high yield via the reductive etherification of furfural in ethanol over Pd/C under mild conditions
复制标题
在温和条件下，通过 Pd/C 上的乙醇中的糠醛还原醚化，轻松高产率合成糠基乙醚
DOI：
10.1039/c7gc03887a
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发表时间：
2018-05-07
期刊：
影响因子：
9.8
通讯作者：
Wu, Peng
中科院分区：
文献类型：
--
作者：
Wang, Yun;Cui, Qianqian;Wu, Peng
系统地研究了以二氧化钛、三氧化二铝、二氧化硅和活性碳为载体的钯纳米粒子在乙醇中催化还原醚化一锅法合成呋喃乙醚的反应。在温和的反应条件下，二氧化硅、二氧化钛和活性碳负载的Pd纳米粒子均具有催化活性，其中Pd/C表现出最高的FEY选择性。考察了钯负载量、反应温度和氢气压力对Pd/C催化剂活性和选择性的影响。结果表明，适宜的Pd用量、较低的反应温度(约60℃)、较低的氢气压力(约0.3 Mpa)有利于乙醚的生成。在优化的反应条件下，首次获得了高达81%的产率，主要副产物为呋喃醇和2-甲基四氢呋喃。与传统的以糠醇为反应中间体的加氢醚化路线相比，还原醚化反应所需的反应温度低得多，在产品收率方面显示出明显的优势。
The one-pot synthesis of furfuryl ethyl ether (FEE) over Pd nanoparticles supported on TiO2, Al2O3, SiO2, and active carbon via the catalytic reductive etherification of furfural in ethanol was systematically studied. The Pd nanoparticles supported on SiO2, TiO2 and active carbon are all active for this novel process under mild reaction conditions, with Pd/C showing the highest selectivity to FEE. The effects of palladium loading, reaction temperature, and hydrogen pressure on the activity and selectivity of Pd/C have been investigated in detail. The results demonstrate that suitable Pd amount, low reaction temperature of about 60 °C, and low H2 pressure of about 0.3 MPa are favorable for the formation of the desired ether product. Under the optimized conditions, an unprecedented high yield of up to 81% of FEE was firstly obtained with the major by-products being furfuryl alcohol and 2-methyltetrahydrofuran. Compared with the conventional hydrogenation-etherification route via furfural alcohol as a reaction intermediate, the reductive etherification shows significant advantage in product yield because of its much lower reaction temperature that is required.