超临界条件下卤素交换氟化制备对氟苯甲醛  

Synthesis of 4-Fluorobenzaldehyde by Halogen Exchange Fluorination in Supercritical Carbon Dioxide

作　　者：吕早生[1] 帅清昱[1] 张路平[1] 武燕娟[1] 任肖丽[1] 陶康[1] 

机构地区：[1]武汉科技大学化学工程与技术学院,湖北武汉430081

出　　处：《化学与生物工程》2014年第6期28-30,共3页Chemistry & Bioengineering

基　　金：高等学校博士学科点专项科研基金联合资助项目(20104219110003)

摘　　要：在超临界条件下用卤素交换氟化的方法制备对氟苯甲醛,研究了助溶剂种类、反应时间、原料物质的量比、反应温度、反应压力等对对氟苯甲醛收率的影响。结果表明:在超临界二氧化碳(scCO2)介质中,以对氯苯甲醛(PCAD)和四丁基氟化铵(TBAF)为原料、以甲醇为助溶剂、以四苯基溴化膦(Ph4PBr)为相转移催化剂,在反应时间为4h、n(TBAF)∶n(PCAD)∶n(Ph4PBr)=1.5∶1∶0.1、反应温度为120℃、反应压力为9.0MPa的优化条件下,对氟苯甲醛的收率达到48.1%。4-Fluorobenzaldehyde was prepared by halogen exchange fluorination of 4-chlorobenzaldehyde（PCAD） with tetrabutylammonium fluoride（TBAF）, using methanol as co-solvent and Ph4 PBr as phase-transfer catalyst in supercritical carbon dioxide. The effects of type of co-solvent,reaction time,material molar ratio, reaction temperature,reaction pressure on the yield of 4-fluorobenzaldehyde were studied in detail. The optimal reaction conditions were obtained as follows：reaction time of 4 h,n（TBAF） ： n（PCAD）： n（Ph4PBr）=l. 5： 1 ： 0.1 ,reaction temperature of 120℃ ,reaction pressure of 9.0 MPa. Under above conditions,the yield of 4-fluorobenzaldehyde reached 48.1%.

关 键 词：超临界二氧化碳 卤素交换氟化 对氟苯甲醛 相转移催化 

分 类 号：TQ244.1[化学工程—有机化工]