苯并咪唑的光催化一步合成及表征

Synthesis of benzimidazole in one step via TiO_2-mediated photocatalysis and its characterization

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%.