基于MCM-41微反应器的微波辅助合成新方法研究有机化学.pdfVIP

2011 年第 31 卷 有 机 化 学 Vol. 31, 2011 第 5 期, 690～694 Chinese Journal of Organic Chemistry No. 5, 690～694 ·研究论文· 基于 MCM-41 微反应器的微波辅助合成新方法研究 * 肖尚友 杨昊书 李倩倩 邱 静 夏之宁 (重庆大学化学化工学院 重庆 400030) 摘要 采用微波辐射合成法合成了纳米介孔分子筛 MCM-41 作为微反应 . 以苯并呋喃-2(3H)-酮的合成为实例, 在甲 苯介质中将邻羟基苯乙酸组装到 MCM-41 微反应器中, 研究了溶液体系及微反应器中反应温度、反应时间及微波辐射 时间对反应的影响. 结果显示, 在施加微波与不施加微波情况下, MCM-41 微反应器中进行的反应较溶液体系中进行的 反应产率提高了 2～33 与 2～12 倍. 对于 MCM-41 微反应器中的反应, 施加微波辐射后反应产率可进一步提高 20%～ 100%. 关键词 MCM-41; 微反应 ; 邻羟基苯乙酸; 苯并呋喃-2(3H)-酮 Investigation on Novel Microwave-Assisted Synthesis Method Based on MCM-41 Microreactor Xiao, Shangyou* Yang, Haoshu Li, Qianqian Qiu, Jing Xia, Zhining (College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030) Abstract MCM-41 mesoporous molecular sieve was synthesized under microwave irradiation and used as microreactor. 2-Hydroxyphenylacetic acid was assembled into MCM-41 microreactor in toluene solution, and benzofuran-2(3H)-one was obtained by the intramolecular esterification of 2-hydroxyphenylacetic acid with high selectivity. The reaction conditions including temperature, reaction time, microwave irradiation and so on were investigated. The yield of benzofuran-2(3H)-one was improved by 2～12 and 2～33 times in MCM-41 microreactor than that in solution under conventional heating and microwave irradiation respec- tively. In addition, the yield of the reaction in MCM-41 reactor under microwave irradiation could be im- proved by 20%～100%. Keyword