无溶剂合成1,3,5-三芳基-2-芳酰基环己醇衍生物和晶体结构有机化学.pdfVIP

2011 年第 31 卷 有 机 化 学 Vol. 31, 2011 第 7 期, 1064～1068 Chinese Journal of Organic Chemistry No. 7, 1064～1068 ·研究论文· 无溶剂合成 1,3,5-三芳基-2-芳酰基环己醇衍生物和晶体结构 刁晓菊 a 季红楼 b 殷 姗 b 荣良策*,b 屠树江 b (a 徐州医学院 徐州 221004) (b 徐州师范大学化学化工学院 徐州 221116) 摘要 在 NaOH 存在下室温研磨查尔酮与丙二腈, 可以有效地得到 1,3,5-三芳基-2-芳酰基环己醇衍生物, 本合成方法 反应时间短、操作简单、产率高, 符合绿色化学特点. 产物结构经过红外、核磁、元素分析和高分辨质谱确证, 并对 3b 做了单晶衍射测定. 关键词 查尔酮; 丙二腈; 无溶剂; 研磨; 环境友好 Synthesis of 1,3,5-Triaryl-2-aroylcyclohexanol Derivatives and Crys- tal Structure under Solvent-Free Conditions Diao, Xiaojua Ji, Hongloub Yin, Shanb Rong, Liangce*,b Tu, Shujiangb a ( Xuzhou Medical College , Xuzhou 221004) (b College of Chemistry and Chemical Engineering, Xuzhou Normal University , Xuzhou 221116) Abstracts An efficient synthesis of 1,3,5-triaryl-2-aroylcyclohexanol derivatives from chalcone and malononitrile was reported in the presence of sodium hydroxide under solvent-free conditions at room tem- perature. The advantages of this procedure were simple protocol, high yields and environment friendliness. 1 Their structures were determined by IR, H NMR spectra, elemental analysis and HRMS spectra, and 3b was additionally confirmed by X-ray diffraction analysis. Keywords chalcone; malononitrile; solvent-free; grinding; environment friendliness 近年来, 无溶剂有机合成反应的报道呈快速增长趋 芳酮分子间缩合、加成、环化反应[5]; (2)硝基甲烷与 α,β - 势[1～3]. 因为它完全克服了有机溶剂带来的易燃、易爆、