With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.76857-14-2,Sodium 3-oxido-5-sulfidoisothiazole-4-carboxylate,as a common compound, the synthetic route is as follows.,76857-14-2
The second intermediate obtained in step (4) is added in portions to the aqueous solution of 4-carboxy-3-hydroxy-5-mercaptoisothiazole trisodium in acetone at a low temperature of 2 to 8C.Then, the pH of the mixed solution was adjusted with sodium bicarbonate to be 7.5 to 9, and allowed to react at 15 to 30 C. and a stirring rate of 30 to 80 r/min for 3 to 8 hours.After filtering, the filter cake is washed with a small amount of deionized water to neutrality, and then dried under reduced pressure to obtain crude cefotetan acid; The cefotetan acid crude product obtained in step (5) is configured as an aqueous acetone suspension, and the excess sodium bicarbonate is stirred and dissolved in batch at room temperature.Then use activated carbon to stir for more than 1h, filter, -5 ~ 5 C,Stir and add 5 ~ 8mol/L hydrochloric acid solution to adjust the pH to less than 3, stir, filter and dry to obtain purified cefotetanic acid; The method for adding sodium bicarbonate is as follows: first, sodium bicarbonate is added in an amount of 30 to 50 g per batch, and after each batch is added,After stirring for 1-3 hours to dissolve, add the next batch, and so on, until the added sodium bicarbonate does not dissolve; At a low temperature of -5 to 10C, cefotetan obtained in step (6) is dissolved in purified water, and then sodium bicarbonate is added in portions.Stir and dissolve and adjust the pH of the solution to below 6, then add the activated carbon to stir for more than 1h, filter,The filtrate is first filtered through a 0.25 mum nylon filter and then filtered through a 0.2-0.3 mum filter.Finally, it is filtered through a nanofiltration membrane of 10 to 50 nm, then sterilized in a sterilization chamber, and freeze-dried at -40 C. to -15 C. for more than 12 hours to obtain the disodium cefotetan.
76857-14-2 Sodium 3-oxido-5-sulfidoisothiazole-4-carboxylate 136151974, aisothiazole compound, is more and more widely used in various fields.
Reference£º
Patent; Jiangsu Han Sitong Pharmaceutical Co., Ltd.; Wang Duoping; Wei Genghu; Shi Jiagui; Lu Lihuan; (9 pag.)CN107540694; (2018); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com