摘要
以全氟碘丁烷为原料,分别与4-碘硝基苯和4-碘苯甲酸反应合成了4-全氟丁基硝基苯(1)和4-全氟丁基苯甲酸(3);1经还原反应,3经酰氯化反应,后再缩合反应制得氟代苯基异羟肟酸(5);5经络合反应合成了氟代苯基异羟肟酸钴(6),其结构经UV-Vis,1H NMR,FT-IR和HR-MS(EI)表征。在氟两相中考察了其对乙苯氧化的催化性能。结果表明:在全氟己烷中,6 0.04 mmol,于60℃反应6 h,乙苯的转化率为49.2%,苯乙酮的选择性为88.3%。6循环使用5次,选择性保持良好。
p-Perfluorohexyl nitrobenzene（1） and p-perfluorohexyl acid（3） were synthesized by reaction of perfluorobutyl iodide with 4-iodonitrobenzene and 4-iodobenzoic acid respectively. Fluoro- phenyl hydroxamic acid（5） was prepared by condensation reaction of the reduction product of 1 with acyl chloride product of 3. The hydroxamic aic-containing cobalt perfluorohexyl chain complexes（6） was synthesized by complexation reaction of 5. The structure was characterized by UV-Vis,1H NMR,FTIR and HR-MS（EI）. Its catalytic activity for the oxidation of ethylbenzene It was investgated. The results indicated that the amount of catalyst was 0. 04 mmol and the reaction was carried out at 60 ℃ for6 h,the conversion of ethyl benzene was up to 49. 2% and the selection of acetophenone was 88. 3%under the conditions of perfluorohexane as solvent. The selectivity of catalyst can maintain good after recycling for five times.
出处
《合成化学》
CAS
CSCD
2016年第9期780-784,共5页
Chinese Journal of Synthetic Chemistry
基金
国家自然科学基金资助项目(21276030)
关键词
氟代苯基异羟肟酸钴
氟两相催化
乙苯氧化
合成
催化性能
fluoro-phenyl hydroxamic acid cobalt
fluorocarbon catalysis
oxidation of ethyl benzene
synthesis
catalytic activity
