A kind of salt-forming method of tianuptine sodium
A technology of tianeptine sodium and tianeptine acid, applied in the direction of organic chemistry and the like, can solve the problems of high equipment requirements, high energy consumption, unsuitable for industrial production and the like, and achieves simple equipment requirements and low reaction conditions. , The production process is simple and controllable
Active Publication Date: 2019-02-12
山东诚汇双达药业有限公司
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Problems solved by technology
[0003] In the recently reported synthesis process of tianuptine sodium, there are generally two methods, one is to hydrolyze the precursor ester of tianuptine acid to form a salt at the same time, such as published by Zhang Guolong of Wuhan Engineering University, etc. "Synthesis of Thienuptine Sodium" (Fine Chemical Intermediates, Issue 10, 2012, Volume 42, Issue 5) and "New Synthesis Process of Antidepressant Thienuptine Sodium" published by Zhang Xiulan of Wuhan Engineering University, etc. "(Guangdong Chemical Industry, No. 2, 2013, Vol. 40, No. 244) is the same. After hydrolysis, the solvent is evaporated to obtain crude salt, and then refined. The disadvantage is that salt formation and hydrolysis are carried out at the same time. , after the reaction, the crude product is an oily viscous substance, which requires repeated recrystallization to obtain a solid product, and the product purity and yield cannot be guaranteed; Sodium hydroxide is salted in water, and the resulting aqueous solution is freeze-dried or spray-dried to obtain the finished product. This method has high purity and yield, but its disadvantages are high requirements for equipment and energy consumption in the production process. Large, high cost, not suitable for industrial production
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Embodiment 1
[0021] Add 43.7g of tianuptine acid to 175g of methanol, add 5.4g of sodium methoxide, stir until clarification, add activated carbon for decolorization, filter, and concentrate the filtrate to dryness at 40-45°C; add 88g of dichloromethane and 2.2g of Dissolve the material in ionized water, then add 44g of ethyl acetate to crystallize at 5-10°C, filter, and dry at 45-50°C under vacuum to obtain 44.1g of tianuptine sodium, with a liquid phase purity of >99.5% and a molar yield of 96.1 %. The detection map is as shown in the attached picture of the instruction manual figure 1 shown.
Embodiment 2
[0023] Add 43.7g of tianuptine acid to 262g of methanol, add 5.4g of sodium methoxide, stir until clear, add activated carbon for decolorization, filter, and concentrate the filtrate to dryness at 40-45°C; add 132g of dichloromethane and 2.2g of Dissolve the material in ionized water, then add 66g of ethyl acetate for crystallization at 5-10°C, filter, and dry at 45-50°C under vacuum to obtain 43.7g of tianuptine sodium, with a liquid phase purity > 99.5%, molar yield The rate is 95.2%.
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The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for salting tianeptine sodium. The method comprises the following steps: adding 7-[(3-chloro-6,11-dihydro-5,5-dioxo-6-methyl dibenzo[c,f][1,2] thiazole-11-yl) amino] heptylic acid into an organic solvent, adding a salting agent to react, after the reaction is completed, adding activated carbon for decoloring treatment, and concentrating till the organic solvent is fully removed; further adding another organic solvent and a proper amount of deionized water for dissolving, adding a crystallization reagent for crystallization, filtering, and drying, thereby obtaining tianeptine sodium. The method provided by the invention is low in reaction condition requirement, simple in equipment, simple and controllable in production process and relatively applicable to industrial production.
Description
technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a salt-forming method of tianuptine sodium. Background technique [0002] The trade name of tianuptine sodium is Datilang, and the chemical name is 7-[(3-chloro-6,11-dihydro-6-methyldibenzo[c,f][1,2]-sulfuron Zazen-11-yl)-amino]heptanoic acid S,S-dioxide sodium salt; a drug for the treatment of mental disorders produced by the French Servier International Company. This product was imported and registered in China in December 2001. It is used for the treatment of mild, moderate or severe depression, neurogenic and reactive depression, anxiety and depression of the body, especially gastrointestinal discomfort, etc. Associated anxiety disorders play a role. Tianuptine sodium is a 5-HT reuptake agonist, which can regulate the remodeling of hippocampus, amygdala and cell dendrites. It has a low incidence of side effects and is a safe and effective antidepressa...
Claims
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IPC IPC(8): C07D281/02
CPCC07D281/02
Inventor 刘志文王庭见杨彦军刘浩李跃东
Owner 山东诚汇双达药业有限公司