Study On The Process Of 11β-Hydroxypregna-1, 4, 16-triene-3, 20-dione Synthesis

Dexamethason is a kind of drug of Steroid Hormon and has many merits, such as anti-sgnail, anti-irritability and anti-shock.11β-Hydroxypregna-1,4,16-triene-3,20- dione(HTD)is a intermediate of dexamethason,and has a prominence influence on the quality and cost of dexamethason.In this thesis the technology of HTD synthesis was systematical studied.This paper performs the yield and conversion ratio and makes a study on the synthesis on HTD. The impact of reaction temperature, size of chromium, concentration of hydrochloric acid, reactant proportion, flow rate and purity of nitrogen, agitation intensity, volume of alcohol and reaction time were investigated, and a optimal synthesize technology was got.The essence of the reaction of chromium with hydrochloric acid was checked by spectrophotometry. The control step was abtained, and a proper reactive model according to the control step was selected. The key factor to accelerate the reaction was checked.HTD is synthesized from 16α,17α–epoxypregna-11α-hydroxy -1,4-diene-3,20– dione(HTD)in industry. According to the similarity in the molecular and crystal structures of HTD and EHDD, the hypothesis of solid solution of the two steroids when they were crystallized from solution were postulated and then confirmed based on the X-ray diffraction, thermal analysis and HPLC of the prepared HTD/EHDD solid solution crystals.The paper supplied a basis for further research and synthesize technology. There is no similar report to above study result has been published in literature up to date.