微波促进的取代酚类化合物的邻甲酰化反应研究  

Research on Microwave Accelerated Ortho-formylation Reactions of Substituted Phenols

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作  者:曾竟[1] 李佳佳[1] ZENG Jing;LI Jia-jia(College of Chemistry and Chemical Engineering,Xinjiang Normal University,Urumqi 830000,China)

机构地区:[1]新疆师范大学化学化工学院,新疆乌鲁木齐830000

出  处:《合成化学》2018年第12期930-933,共4页Chinese Journal of Synthetic Chemistry

基  金:新疆师范大学博士启动基金资助项目(XJNUBS1508)

摘  要:以4-氯苯酚(1a)为原料,研究了微波促进的取代酚类化合物的邻甲酰化反应。考察了催化剂种类及其用量、溶剂、1a与多聚甲醛摩尔比(r)、微波辐射功率和辐射时间等对反应的影响。结果表明:以THF为溶剂,MgCl2/Et3N(2. 5 eq.)为催化剂,r=1/5,在400 W微波功率下辐射反应5 min,5-氯-2-羟基苯甲醛(2a)的产率为85%,其结构经1H NMR确证。该反应条件还适用于多种取代酚(1b~1f)的邻甲酰化反应,产率为78%~90%。Microwave accelerated o-formylation reactions of substituted phenols was discussed by using4-chloro phenol(1a)as the material.Effects of catalysts type and amount,solvents,molar ratio(r)of1a and paraformaldehyde,reaction time and the power of microwave radiation on the reaction were investigated.The experimental results indicated that MgCl2/Et3N(2.5eq.)as catalyst,r=1/5,THF as solvent,microwave radiation at400W for5min,the yield of5-chloro-2-hydroxybenzaldehyde(2a)was85%.The structure was confirmed by^1H NMR.Besides,this reaction conditions also suited to ortho-formylation of other phenols(1b^1f)and showed a remarkable tolerance toward different functional groups.The yields were78%~90%.

关 键 词:取代酚 邻甲酰化 取代水杨醛 合成 微波促进 

分 类 号:O621[理学—有机化学]

 

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