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以对二硝基苯(PDNB)为反应底物,以高活性的无水四丁基氟化铵(TBAFanh.)为氟化剂,经氟代脱硝法一步合成了对硝基氟苯(PNFB),研究了溶剂用量、原料摩尔比、反应时间、反应介质以及氟化剂种类等因素对反应的影响。得出最佳合成工艺条件为:n(PDNB)∶n(TBAFanh.)=1∶1.2,TBAFanh.30 mmol、PDNB 25 mmol、无水四氢呋喃(THF)10 mL、于室温反应1.5 h,对硝基氟苯收率可达98.5%,色谱纯度99.0%以上。并在优化条件下进行了3次平行实验,重复性良好。反应具有条件温和、产物收率高和副反应少等优点。
Using p-nitrobenzene (PDNB) as the reaction substrate and high activity anhydrous tetrabutylammonium fluoride (TBAFanh.) As the fluorinating agent, p-nitrofluorobenzene (PNFB ), The effects of solvent dosage, molar ratio of raw materials, reaction time, reaction medium and the kind of fluorination agent on the reaction were studied. The optimum synthesis conditions were as follows: n (PDNB): n (TBAFanh.) = 1: 1.2, TBAFanh.30 mmol, PDNB 25 mmol and anhydrous THF Fluorobenzene yield up to 98.5%, chromatographic purity of 99.0% or more. Under the optimal conditions, three parallel experiments were performed with good repeatability. The reaction has the advantages of mild conditions, high product yield and few side reactions.