实验技术与管理
實驗技術與管理
실험기술여관리
EXPERIMENTAL TECHNOLOGY AND MANAGEMENT
2014年
7期
39-42
,共4页
章建东%孙辉%姜文清%李亚红
章建東%孫輝%薑文清%李亞紅
장건동%손휘%강문청%리아홍
Knoevenagel缩合反应%分子筛固载氟化钾%丙二腈%氰乙酸乙酯%绿色合成
Knoevenagel縮閤反應%分子篩固載氟化鉀%丙二腈%氰乙痠乙酯%綠色閤成
Knoevenagel축합반응%분자사고재불화갑%병이정%청을산을지%록색합성
Knoevenagel condensation reaction%KF supported on molecular sieve%malononitrile%ethyl cyanocaetate%green synthesis
室温下以分子筛固载氟化钾为催化剂催化芳香醛和丙二腈(或氰乙酸乙酯)的Knoevenagel缩合反应,合成了一系列的不饱和产物。考察了原料和催化剂的用量对产率的影响,利用薄板层析(T LC )确定反应时间。最佳合成条件是芳醛和丙二腈(或氰乙酸乙酯)的物质的量比为5∶5.5,催化剂用量为0.30g,室温反应45~300 min ,产率可达87%~99%。该反应具有操作和后处理方便、产率高、污染少等优点。另外,催化剂通过简单的处理即可循环使用,为该化合物的制备提供了简便易行的方法,既可强化学生的环保意识,又可使学生掌握绿色化学的实用技术。
室溫下以分子篩固載氟化鉀為催化劑催化芳香醛和丙二腈(或氰乙痠乙酯)的Knoevenagel縮閤反應,閤成瞭一繫列的不飽和產物。攷察瞭原料和催化劑的用量對產率的影響,利用薄闆層析(T LC )確定反應時間。最佳閤成條件是芳醛和丙二腈(或氰乙痠乙酯)的物質的量比為5∶5.5,催化劑用量為0.30g,室溫反應45~300 min ,產率可達87%~99%。該反應具有操作和後處理方便、產率高、汙染少等優點。另外,催化劑通過簡單的處理即可循環使用,為該化閤物的製備提供瞭簡便易行的方法,既可彊化學生的環保意識,又可使學生掌握綠色化學的實用技術。
실온하이분자사고재불화갑위최화제최화방향철화병이정(혹청을산을지)적Knoevenagel축합반응,합성료일계렬적불포화산물。고찰료원료화최화제적용량대산솔적영향,이용박판층석(T LC )학정반응시간。최가합성조건시방철화병이정(혹청을산을지)적물질적량비위5∶5.5,최화제용량위0.30g,실온반응45~300 min ,산솔가체87%~99%。해반응구유조작화후처리방편、산솔고、오염소등우점。령외,최화제통과간단적처리즉가순배사용,위해화합물적제비제공료간편역행적방법,기가강화학생적배보의식,우가사학생장악록색화학적실용기술。
KF supported on molecular sieve is used as the catalyst for the Knoevenagel condensation reaction of aromatic aldehydes with malononitrile or ethyl cyanoacetate at room temperature . A series of unsaturated products are synthesized .Effects of the amount of raw materials and the catalyst loadings on the yields are investigated ,and the reaction times are determined by thin layer chromatography (TLC ) . The optimum reaction conditions are as follows :the molar ratio of aromatic aldehydes to malononitrile or ethyl cyanoacetate is 5∶5 .5 ,the amount of the catalyst is 0 .3 g and the reaction time at room temperature is 45-300 min .The yield of products reaches 81~93% .This method possesses the advantages of simple operation and work-up procedure ,good yields and less pollution .The catalyst can be recycled by simple treatment .This reaction provides a simple and easy method for the preparation of the compounds .Using this method ,students can raise their consciousness of environmental protection and master practical teaching techniques of green-chemistry .