2-(5-硝基苯并咪唑基)乙腈合成工艺探讨

Technological Process of the Synthesis of 2-( 5-nitrobenzimidazole) acetonitrile

目的通过正交试验法优化目标产物2-(5-硝基苯并咪唑基)乙腈合成工艺条件。方法根据3因素4水平正交试验设计,以5-硝基苯并咪唑和氯乙腈为原料,通过亲核取代反应合成目标产物,以反应转化率为指标,优化实验条件。目标化合物通过IR、1HNMR进行结构表征。结果以氢氧化钾为缚酸剂,乙酸乙酯为溶剂,反应时间8h,得到的目标化合物总得率最高(79.9%),且后处理简单。结论通过正交试验法优化2-(5-硝基苯并咪唑基)乙腈的合成,所得产物产率高、纯度好。

OBJECTIVE To optimized condition on the synthesis of 2-（ 5-nitro-benzimidazole ） acetonitrile by orthogonal experiment.METHODS According to L9 （34 ） orthogonal experiment design,the target product 2-（5-ni-troben-zimidazole） acetonitrile was synthesized from the nucleophilic substitution reaction of 5-nitrobenzimidazole and chloroacetonitrile.Optimized experimental condition base on reaction conversion rate index,and the structure of syn-thetic compound determined by IR、1 H-NMR analysis.RESULTS The target compound had the higher rate （79.9%） with potassium hydroxide as bound acid,ethyl acetate as solvent,the reaction time was 8h,and the post-processing was simple.CONCLUSION The synthesis of target compound 2-（5-nitrobenzimidazole） acetonitrile by orthogonal experiment is high yield and good purity.