Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.98827-44-2,A new synthetic method of this compound is introduced below.98827-44-2
260 kg of 4-hydroxy-2H-thieno [2,3-e] -1,2-thiazine-3-carboxylic acid methyl ester 1,1-dioxide were dissolved in500kgDMF, add potassium carbonate 150kg, warmed to 140 C, and dropping 120kg of dimethyl carbonate, 2h drop end, after the dropwise addition, the reaction was continued for 5h, then add 140kg of potassium carbonate, dropping 300 kg of 2 – aminopyridine in dimethylformamide (DMF) (120kg 2-aminopyridine dissolved in 180 kg DMF), 2h addition was complete, the reaction was continued for 5h. After the reaction, cooling and filtering to remove potassium carbonate, the filtrate was recovered under reduced pressure most of the DMF, the residue was added mass concentration of 3% sodium hydroxide alkaline water, activated carbon bleaching, filtration, the filtrate was purified hydrochloric acid to pH = 3 -4, precipitated yellowish solid, centrifuged, the material was washed until neutral, dried, to give a yellow solid 276kg, yield 83%, product purity 99.85%.
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Reference£º
Patent; Jiangsu Engineering Polytechnic College; Yan Bin; Feng Chengliang; Guo Liqiang; (5 pag.)CN106916169; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem