摘要
通过亲核取代合成了9种[Ph_3PR]^+-型季鏻盐,并通过红外、核磁氢谱进行了表征。将合成的季鏻盐作为相转移催化剂用于卤素交换氟化合成对氟硝基苯的反应,结果表明,在9种季鏻盐中,[Ph_3PC_4H_9]^+Br-的催化性能最佳。考察了催化剂用量、时间、KF用量、温度、溶剂等因素对反应的影响,得到的最优工艺条件为m(季鏻盐)∶m(KF)=0.02,n(KF)∶n(对氯硝基苯)=2,温度190℃,时间3h,溶剂为二甲基亚砜;在此条件下原料转化率为95.63%,产物收率90.89%。
Nine kinds[Ph_3PR]^＋X^-quaternary phosphonium salts which were synthesized through nucleophilic substitution method were characterized by IR,^1 H NMR.These quaternary phosphonium salts as phase transfer catalysts for the synthesis of fluoronitrobenzene through the halogen exchange fluorination reaction.Results showed that in these nine kinds quaternary phosphonium salts,[Ph_3PC_4H_9]^＋Br^-had the best catalytic performance.Also,the effect of yeid of the amount of catalyst,time,KF dosage,temperature and solvents for the reaction were studied.The optimal conditions were as follows：m（quaternary phosphonium salt）∶m（KF）=0.02,n（KF）∶n（chloronitrobenzene）=2,the temperature was 190 ℃,the time was 3hours,the solvent was dimethyl sulfoxide;Under which condition,the conversion was 95.63%,the reaction yeild was 90.89%.
出处
《精细石油化工》
CAS
CSCD
北大核心
2016年第4期38-42,共5页
Speciality Petrochemicals
关键词
季鏻盐
相转移催化
对氟硝基苯
quaternary phosphonium salt
phase transfer catalysis
fluoronitrobenzene
