摘要
以2-吡啶甲酸与邻苯二胺为原料,分别采用两种不同的方法合成了标题化合物。研究表明,亚磷酸三苯酯法具有操作简便、所得产品纯度高等特点。通过正交试验优化的反应条件为:反应温度120℃,反应时间3h,n(亚磷酸三苯酯):n(2-吡啶甲酸)=0.67:1,收率为82.5%。产品经HPLC分析,含量99.7%。化合物结构经MS、IR、1HNMR确证。
1,2-Bis（2-pyridinecarboxamido）benzene was synthesized from 2-pyridinecarboxylic acid and 1,2-diaminobenzene by two different methods.The results showed that the method of triphenyl phosphite had many advantages,such as easiness of operation and high purity of the product.The factors affecting synthesis process were studied in detail by means of orthogonal tests.The optimum conditions were obtained as follows：a molar ratio of triphenyl phosphite and 2-pyridinecarboxylic acid at 0.67∶1,a reaction temperature of 120 ℃ and a reaction time of 3 h.The product was characterized by IR,MS and ^1HNMR.The purity of the product was 99.7% and the yield was 82.5%.
出处
《化学试剂》
CAS
CSCD
北大核心
2008年第6期440-442,共3页
Chemical Reagents
基金
浙江省教育厅科研项目(20061237)
