Process Optimization Of The Dezocine API Intermediates Synthesis Technology

In this thesis, the synthetic process of Dezocine-VI (1-(5-bromo pentane)-7-methoxy-l-methyl four hydrogen naphthyl ketone) and Dezocine-VIII (5,6,7,8,9,10,11,12-eight hydrogen-3-methoxyl-5,11-methylene benzene and ring decene-13-ketoxime) were studied, which were the intermediates of the API of Dezocine Injection produced by Yangtze River Pharmaceutical Group Company Limited. The yelds or contents of the synthetic processes were studied through single factor experiment, and the synthetic conditions were optimized by small experiments. The research contents were as follows:(1) The synthetic process of Dezocine-VI (1-(5-bromo pentane)-7-methoxy-1-methyl four hydrogen naphthyl ketone) was optimized through analysis of process capacity and evaluation of influencing factors. The influence laws of the temperature, time and dropping speed of35%sodium hydroxide to the content were studied, and the optimal synthetic process was selected by orthogonal tests.(2) The synthetic process of Dezocine-VIII (5,6,7,8,9,10,11,12-eight hydrogen-3-methoxyl-5,11-methylene benzene and ring decene-13-ketoxime) was optimized through analysis of process capacity and evaluation of influencing factors. The influence laws of the temperature, time and ratio of hydrochloric acid and alkali to the content were studied, and the optimal synthetic process was selected by orthogonal tests.(3) The reliability of the synthetic conditions selected by small experiments was verified by batch production, which would provide basic data to the scale change of the synthetic process.