1446750-99-7Relevant articles and documents
Preparation method of vortioxetine hydrobromide impurity standard substance
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Paragraph 0036; 0042-0044; 0049-0050, (2021/01/29)
The invention relates to the technical field of drug impurity standard substances, and discloses a preparation method of a vortioxetine hydrobromide impurity standard substance. The preparation methodcomprises the steps of S1, conducting a condensation reaction, specifically, adding o-phenylenediamine, bis(2-chloroethyl) amine hydrochloric acid and an organic solvent into a reaction flask, stirring for reflux reaction, stopping heating, stirring for cooling, adding methanol into the reaction solution, stirring for dissolution, adding diethyl ether into the reaction bottle, separating out a large amount of brown solid, filtering, transferring the solid into the reaction bottle, adding 2N sodium hydroxide solution, stirring, extracting by using ethyl acetate, collecting an organic layer, drying, filtering and concentrating to obtain a 1,2-bis(piperazin-1-yl) benzene crude product and a brown oily substance. The 1,2-bis(piperazine-1-yl) benzene preparation process is simple, short in synthesis period, low in synthesis cost and novel in refining method, is suitable for small-amount synthesis in laboratories and can also be used for large-scale production, the 1,2-bis(piperazine-1-yl)benzene content calibration method is a conventional analysis method, and the equipment is conventional equipment and is easy to realize.