Hesperidin Derivatives Technology

Methylhesperidin, well- water-soluble, well-oral-absorption and high rate of biologic utilization medicine, belongs to a kind of Vp, which is used to strength the resistance on capillary tube, to prevent from disturbing blood vessel which arteriosclerosis causes. With population aging and the increasing prevalence rate of cardiovascular disease, as a cardinal content of a drug, which is used to treat with cardiovascular disease, the market value of methylhesperidin is higher.At present, the production technology and condition, production rate of methylhesperidin in abroad has not been reported. The production conditions are kept secret from external, and the production has been abnormal in two domestic factories, where methylhesperidin is yielded. The supply is unable to meet the demand. There is only a reference where the method of synthesizing methylhesperidin, that hesperidin, botanic extract, is methylated by the dimethylsulfate, is mentioned curtly. This research is the study of every technology conditions during yielding methylhesperidin, the estimate of technology condition influencing the production, so as to ascertain the best production conditions and provide the related data for subsequent experiment. Altering the density of alkali and investigating the technology conditions in the course of the reaction, the separation, the concentration and the crystal are adopted to optimum condition of technology, and to improve the yield and the quality of methylhesperidin. Based on complete researches, orthogonal experiment is designed by combining the density of alkali, reaction temperature, the useful quantity and the adding rate of dimethylsulfate, stirring time and condensing substance. The better conditions of technology are that the density of alkali is 5%, reaction temperature is 30℃, the useful quantity of dimethylsulfate is quadruple quantity on theory, the adding rate of dimethylsulfate is quicker, stirring time is 3 hours, condensing substance is saturated limewater. According to the new reaction condition of technology, the yield of product increase 4.07%.Combining the useful quantity of butyl alcohol and recovering butyl alcohol, extracting times design orthogonal experiment. The best conditions of technology are that the useful quantity of butyl alcohol is 25 times quantity of material, extracting number of times is 5 times, and it does not use recovering butyl alcohol. According to the new condition of technology, the purity of product increase 1.33%.Comparing the ways of relieving pressure and normal pressure stilling to study the influence on product, the result is that the product almost keeps as excellent as before in the method of relieving pressure stilling.This paper confirms the crystallizing effectiveness is better and the time of crystal is shorter under the condition of the freezing than on the normal temperature.The illustrated results on the infrared spectrum and the element analysis proved that the compound is the methylhesperidin. According to The Drugs Standard by SFDA on methylhesperidin, the properties and purity of product were tested and characteristics are in accord with the standard.The topic investigates roundly the technology conditions in the course of the reaction, the separation, the concentration and the crystal, complete perfectly the tasks and gain anticipative ends.