The Synthesis And Characterization Of 3,3’,5,5’-tetramethyl Benzidine And A New Type Of Fluorescent Substance

New chromogenic,fluorescent substance was found and detected with the development of the chemical sensing technology. as the most widely useful color reagent,3,3’,5,5’-tetrame thyl benzidine (TMB) was praised by many experts because of its characteristics such as color visual contrast,no carcinogenicity. But the TMB source mainly rely on imports, domestic am-ounts of production is extremely limited, the prospect of market is quite favorable; as a new ty pe of fluorescent color material,4,5-di(4-dimethyl amino phenyl)-2-(3,5-methoxy-4-hydroxy phenyl)-midazole (MZ),its total synthesis route was not reported in the literature at present. So, the synthesis and characterization of the above two kinds of substance have the important meaning. In the thesis, the following studies were carried out.(1) The synthetic route of TMB has been filtrated and optimized, A synthesis route, in which Protection, bromination, coupling was selected. The synthetic route, although it has mo re steps,it is more suitable for the production status of pilot magnification considering the reaction yield and production cost, and the industrial scale-up. The structure of the final produ ct was confirmed by using the 1H-NMR,MS spectroscopies. the various main steps reaction conditions are optimized in the test experiment and got the ideal yield. According to the optimizing reaction conditions in test experiment, we further optimized condition of the pilot test, maximum reduce the amplification effect and stabilized the pilot yield, the cost, safety and yield of TMB were improved in industrialization, laid a foundation for the pilot product ion. According to the comprehensive data and experience in the former experiment,20batches of production has been carried which further proved the feasibility of the synthesis process and stability.(2) The synthesis route of 4,5-di(4-dimethyl amino phenyl)-2-(3,5-methoxy-4-hydroxy phenyl)-midazole (MZ) was filtrated and optimized. considering cost,operability and other factors, chose the F-K reaction rather than the oxidation and managed to get through the synthesis route, the main factors of the various steps of reaction route has been optimized and improved yield a bit. The structure of the final product also was confirmed by using LC-MS and 1H-NMR spectroscopies, the foundation of theory and practice of industrial production was laid.