Study On Synthesis Of Drospirenone And Purification Technology Of Crude Product

Drospirenone is a kind of high efficiency,low toxicity,no side effects of a new generation of steroidal contraceptives,it is similar to natural progesterone pharmacological properties of pregnant excitation,is a derivative of steroidal 17a spironolactone.In this paper,we were studied about the synthesis process route,purification process and detection system.First,we design a new synthetic route based on the original process route,and then synthesize the experimental study,finally,we design a new chromatography detection system for the detection and characterization of the products.(1)The feasibility of chromium anhydride oxidation process was determined in the study.According to the oxidation process,the synthesis process was optimized,anddesignanew synthetic route,which was safe,environmentally friendly and economical.(2)The experimental study on the synthesis of buspirone shows that the reaction time is 3 h in the synthesis of epoxy resin and the fresh potassium tert butyl alcohol is best to reaction.In the process of esterification,the reaction temperature was set at 80?,the reaction time was about 5 h,the effect of sodium was better than that of potassium.In the process of synthesis,the reaction time was 24 h,and the optimum pH range was 8-8.5 In the course of the synthesis of buspirone the first reaction time was 6 h,and the second reaction time was 2 h?(3)To purify the crude product of the raw materials and to design the on-line monitoring system,we can monitor and control the reaction process in real time.Choice of silica gel as the adsorbent of this experiment;determine the cyclohexane and EA mixed solution as the elution agent,and determine the cyclohexane and EA ratio of 1,the best separation effect.The impurities in the crude product of the raw materials were analyzed,and the types and causes of the impurities were determined.The products are fully analyzed,the results show that the yield of the product,in accordance with the USP36 quality requirements.By IR analysis,element analysis showed that the content of each element in the process of the content of each element in the process of the content of the element and the theory value,indicating that the product did not occur in the solvent immersion.(4)Purification process of comparison,through comparison of pyridine hydrochloride into salt purification process,sodium sulfite-aqueous solution reduction method purification process and study new technique of silica gel column chromatography purification process of three kinds of process of the product obtained from the appearance,the yield and purity of single impurity such as three aspects were compared.The results show that the silica gel column chromatography purification method.The results of the appearance of the product best,purification yield reaches 90.76%and the purity reached 99.84%and the largest single impurity is 0.08%,indicating that the purification process and other process has great advantages compared.The chromatography process is simulated and the results are fitted by GR model,and the influence of the parameters on the results of the chromatography is analyzed,which provides the basis for the industrial amplification.The flexor drospirenone synthesis and purification process of research.The result is industrial production base and put into use in the company,improves the production efficiency of enterprise,reduce the production costs of enterprises.