制备了气相催化氧化2-甲基吡啶合成2-吡啶甲醛的双金属Bi-Mo/TiO_2催化剂,采用XRD、H_2-TPR、SEM和XPS对催化剂进行了表征,并考察了催化剂组成、反应温度、原料流率等因素的影响。实验研究结果表明,Bi-Mo/TiO_2对2-甲基吡啶有比较高的催化活性是基于Bi_2Mo_3O_(12)和MoO_3的协同催化作用,Bi2Mo_3O_(12)和MoO_3的较佳摩尔比率为1:1,催化剂的较佳负载量为15%(wt),低反应温度和高原料流率可以提高对2-吡啶甲醛的选择性。较佳反应条件下(反应温度290℃,10%(wt)2-甲基吡啶水溶液的流率为0.5 m L×min-1,氧气的流率为0.1 L×min^(-1),空速12600 h^(-1)),2-甲基吡啶的转化率为70.9%,2-吡啶甲醛的选择性为83.1%。
An improved synthetic process for 3-benzyloxy-4-n-butylaniline hydrochloride the key intermediate of nequinate which is an anticoccidal drug to parasites of Eimeria,was described.The process was started with 3-aminophenol,via acylation,Fries rearrangement,benzylation,hydrolysis,and Huang-Minlon reduction,to give the title compound.The optimal reaction conditions and molar yield were as follows:acylation,130—140℃ for 3 h;Fries rearrangement,140℃ for 5 h,77.9%(based on 3-aminophenol);benzylation,70℃ for 2 h and 80℃ for 4 h,81.3%;hydrolysis and Huang-Minlon reduction,reflux for 90 min,78.2%.The structures of the main compounds were confirmed by 1H NMR.The process is much of industrial value because of high yields,cheap and available materials,moderate reaction conditions and convenient operations.
