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该文以邻苯二胺和α-甘氨酸为主要合成原料,合成了2-氨基烷基苯并咪唑衍生物的代表化合物2-甲胺基苯并咪唑;探讨了原料摩尔比、反应溶剂、反应温度、反应时间及催化剂种类等因素对反应的影响;采用熔点、红外、元素分析等方法对产物进行了表征。得到了制备2-甲胺基苯并咪唑的最佳反应条件:磷酸和多聚磷酸的混酸为催化剂,该混酸同时作为反应溶剂,反应时间30 h,反应温度190℃,邻苯二胺和相对应的氨基酸的最佳摩尔比为1∶3.5,磷酸和多聚磷酸的摩尔比为1∶2。为了避免中间体的氧化和其他副反应发生,反应过程用氮气保护。在该条件下,目标化合物的合成收率可达85%。该文报道工作的新颖性,已为济南市科技信息研究所2008年9月16日出具的第JN280255号《科技查新报告》所证实。
In this paper, o-phenylenediamine and α-glycine as the main synthetic raw materials, synthesized 2-aminoalkylbenzimidazole derivatives of the representative compound 2-methylaminobenzimidazole; discussed the molar ratio of raw materials, the reaction solvent, the reaction Temperature, reaction time and the type of catalyst on the reaction. The products were characterized by melting point, infrared and elemental analysis. The optimum reaction conditions for the preparation of 2-methylaminobenzimidazole were obtained. The mixed acid of phosphoric acid and polyphosphoric acid was used as the catalyst. The mixed acid was used as the reaction solvent at the same time. The reaction time was 30 h, the reaction temperature was 190 ℃, The optimum molar ratio of the corresponding amino acids is 1: 3.5, and the molar ratio of phosphoric acid to polyphosphoric acid is 1: 2. In order to avoid the oxidation of intermediates and other side reactions, the reaction process is protected with nitrogen. Under this condition, the synthesis yield of the target compound can reach 85%. This article reports the novelty of the work and has been confirmed by the Science and Technology Inspection Report No. JN280255 issued by Jinan Institute of Science and Technology Information on September 16,