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PAGE ii
摘 要
采用浸渍法制备了分子筛催化剂,以分子筛负载七水氯化亚铈制成负载型催化剂。并对其进行XRD、SEM、BET等表征。在无溶剂条件下,考察了其催化2-甲基吲哚与2-环己烯酮的Michael加成反应合成药物中间体3-(2-甲-1H-吲哚-3-基) 环己酮的催化性能。并对产物进行了气相色谱-质谱分析鉴定产物结构和气相色谱分析产物含量,进行了单因素探索实验。结果表明,分子筛比表面积 对催化剂活性影响较大,而分子筛酸性的协同催化效应并不是的那么明显CeCl3/H BEA、CeCl3/H-ZSM-5、CeCl3/H-MCM-41和CeCl3/H-USY 4种催化剂中CeCl3/H-MCM-41表现出高的催化活性。以30%CeCl3/H-MCM-41为催化剂,在2-环己烯酮与2-甲基吲哚的摩尔比1.1、催化剂用量7.5%、反 应温度为80℃、反应时间60 min的条件下,3-(2-甲基-lH-吲哚-3-基)环己酮的产率达到97.5%。 关键词:2-甲基吲哚;2-环己烯酮;分子筛;CeCl3;3-(2-甲基-1H-吲哚-3-基)环己酮
Abstract
The catalysts of supporting on molecular sieves were prepared by impregnation method ,load seven water cerous chloride made supported catalyst with molecular sieve and characterized by XRD,SEM and BET.The catalytic performance of the catalysts for synthesis of 3-(2-methyl-1 H-indol-3-y1) cyclohexanone was examined from the catalytic Mich-eal addition with 2-methylindole and cyclohexenone-2 under solvent free condition.The products were analyzed by gas chromatography-mass spectrometry analysis of the content of the product phase identification structure and gas chromatography.The results indicated that the specific surface area of molecular sieve greatly influenced the catalyst activity,and catalytic synergistic effect with acidity of molecular sieve was not obvious.CeCl3/H-MCM-41 exhibited highest activity among four catalysts of CeCl3/H-BEA,CeCl3/H-ZSM-5,CeCl3/H-MCM-4 l and CeCl3/HUSY.With 30%CeCl3/H-MCM-4 1 as catalyst,under the optimalreaction conditions of catalyst dosage 7.5%,mole ratio of cyclohexenone-2 to 2 methylindole being1∶1 reaction temperature 80℃and reaction time 60 min,the yield of 3-(2-methyl-1H-indol-3-y1) cyclohexanone was up to 97.5%.
Key words:2-methyl indole;2-cyclohexenone;molecular sieve;CeCl3;3-(2-methyl-1H-indol-3-y1)cyclohexanone
目录
TOC \o 1-3 \h \z \u HYPERLINK \l _Toc389999486 摘 要 Ⅰ
HYP
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