26638-53-9Relevant articles and documents
Preparation method of intermediate for preparing tianeptine sodium
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, (2019/09/05)
The invention discloses a preparation method of an intermediate compound for preparing tianeptine sodium. The intermediate compound is shown as a formula. According to the synthesis method, p-chlorotoluene is used as a starting raw material to react with chlorosulfonic acid to obtain sulfonyl chloride, the sulfonyl chloride undergoes an amidation reaction with N-methylaniline under alkaline conditions to obtain sulfonamide, an aqueous solution of the sulfonamide and air are continuously pumped into a fixed bed reactor loaded with an immobilized catalyst according to a certain ration for oxidation to obtain carboxylic acid, and then the carboxylic acid is subjected to cyclization under catalysis of a solid acid to obtain the target compound. The method has simple and few steps, the cost ofthe raw materials is low, the fixed bed reactor and the solid acid catalyst are utilized, the catalyst can be repeatedly recycled to reduce the discharge of the three wastes, the production process isenvironmentally friendly, and the method is more suitable for industrial production.
Preparation method of tianeptine sodium intermediate
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Paragraph 0017, (2016/11/21)
The invention belongs to the technical field of chemical synthesis, in particular relates to a preparation method of a tianeptine sodium intermediate. The preparation method comprises the following steps: adding 2-(N-methyl-N-phenyl-sulfamoyl)-4-chlorine-benzoic acid in an organic solvent, carrying out heating reflux after adding a mixed solution of a chlorinated reagent and the organic solvent, and cooling to room temperature after a reaction is completed; then carrying out heating reflux after adding a mixed solution of a cyclization reagent and the organic solvent; adding a reaction solution in water for hydrolysis after the reaction is completed, layering, extracting with organic solvent, concentrating a mixed organic phase, and adding other solvents for refining so as to obtain the tianeptine sodium intermediate, i.e. 3-chlorine-6-methyl-dibenzo[c,f][1,2] thiazepan-11(6H)-one-5,5-dioxide. According to the preparation method of the tianeptine sodium intermediate, disclosed by the invention, thionyl chloride is adopted as the chlorinated reagent, titanium tetrachloride is adopted as the cyclization reagent, the requirements on reaction conditions are not high, the equipment requirements are simple, a production process is simple and convenient in operation and is safe and controllable, and the preparation method is more suitable for industrial production.