963-75-7Relevant articles and documents
Preparation method of rocuronium bromide intermediate
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Paragraph 0029-0041, (2021/11/26)
The invention belongs to the technical field of drug synthesis, and particularly relates to a preparation method of a rocuronium bromide intermediate. To the preparation method, androsterone as shown I is used as a raw material, dehydration reaction is carried out under catalysis of an ecton reagent, and then washing is carried out. To the preparation method, the reaction temperature is reduced -2 - to -17 - 5 α - the byproduct of high-temperature reaction is reduced 40 °C, the reaction liquid is subjected to simple water washing, extraction and concentration to obtain a white solid, and the loss of the main product caused by the recrystallization of the by-product is reduced. The process is simpler, the yield is lower, and the three-waste discharge is less.
Preparation method of 5alpha-androstane-2-ene-17 ketone
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Paragraph 0025-0030, (2021/11/14)
The invention discloses a preparation method of a skeletal muscle relaxant drug intermediate 5 alpha-androstane-2-ene-17 ketone, and belongs to the technical field of synthesis. According to the method disclosed by the invention, epiandrosterone is taken as a raw material and reacts with p-dodecyl benzene sulfonyl chloride under the action of a catalyst to generate sulfonate, and the 5alpha-androstane-2-ene-17 ketone is generated by elmination. The synthesis method provided by the invention can effectively reduce a double-bond position isomer 5 [alpha]-androstane-3-ene-17 ketone of the target product 5 [alpha]-androstane-2-ene-17 ketone, greatly improves the product quality, and reduces the production cost at the same time.
Preparation method of 5 alpha-androstane-2-ethylene-17-ketone
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Paragraph 0021-0024; 0025-0026; 0027-0028; 0029-0044, (2019/05/08)
The invention discloses a preparation method of 5 alpha-androstane-2-ethylene-17-ketone. The preparation method comprises the steps of taking epiandrosterone (formula I as shown in the specification)as a raw material to give a dehydration reaction by joint catalysis of protonic acid and trifluoromethanesulfonate, and performing post-treatment, recrystallization and separation on a reaction product to form 5 alpha-androstane-2-ethylene-17-ketone (formula II as shown in the specification). The preparation method avoids the use of much organic base compound in the traditional method, has the advantages of high reaction yield, short procedure, good selectivity, low cost, less waste gas, waste water and industrial residue and the like and is a synthesis method suitable for industrial production.