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作 者:王济奎[1] 张友娟[1] 陈国松[1] 陆小华[2]
机构地区:[1]南京工业大学理学院,江苏南京210009 [2]南京工业大学化学化工学院,江苏南京210009
出 处:《化学试剂》2008年第2期115-116,119,共3页Chemical Reagents
基 金:国家杰出青年科学基金(29925616);国家自然科学基金(20246002,20236010);江苏省2003年环保科技计划项目(2003025)资助
摘 要:以邻硝基苯胺和甲醛为原料,超细纳米TiO2为催化剂,利用自制的微型光催化反应器一步合成了标题化合物。与传统方法相比,该法反应条件温和,操作简便,耗时短,产率高。利用熔点测定、红外光谱、核磁共振等手段对合成产物进行了表征。利用高效液相色谱和外标法建立了工作曲线。苯并咪唑浓度在10-200mg/L范围内与峰面积线性关系良好。回收率为98.4%-102.9%,相对标准偏差〈1.87%。A direct one-step synthesis of benzimidazole in methanol from o-nitroaniline and formaldehyde was described using the nano-scale Ti02 as the catalyst. The photocatalytie procedure was carried out in a self-made micro-reactor. Compared to the previously reported methods, this new procedure featured a simple process, mild conditions, good yields and a shorter reaction time. The product was characterized by the melting point determination, IR and NMR. The reversed-phase high performance liquid chromatography and external standard were used to establish the working curve. The analytical results showed that the peak areas exhibited good linearity in compliance with the sample concentration, when the concentration of benzimidazole was (10 - 200) mg/L. The recovery was 98.4% - 102.9%, and the RSD was 〈 1.87%.
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