1003024-00-7Relevant articles and documents
Synthesis and purification method of tildipirosin
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Paragraph 0042-0043; 0048-0049; 0054-0055, (2021/04/21)
The invention discloses a synthesis and purification method of tildipirosin. The method comprises the following steps of dissolving tylosin phosphate in an organic solvent, adding formic acid and piperidine, and performing a heating reaction; performing cooling, adding water and hydrobromic acid, and performing standing for layering; hydrolyzing an aqueous solution A, performing cooling, adding the organic solvent, and performing standing for layering; adding alkali into a water phase to adjust the pH value to 6.5-7.0, adding the organic solvent and alkali to adjust the pH value to be greater than 13, performing standing for layering to obtain a filtrate, and controlling the water content to be less than 0.1% through atmospheric distillation; adding triphenylphosphine and pyridine, performing heating, dropwise adding an iodine solution, continuously reacting, performing cooling, adding alkali for quenching, and performing standing for layering; adding an alkali catalyst and piperidine into the filtrate C, performing a heating reaction, performing cooling, adding acid to adjust the pH value to 6.20-6.80, and performing standing for layering; adding the organic solvent into the water phase, and performing standing for layering; and continuously adding the organic solvent and the alkali into the water phase to adjust the pH value to be greater than 13, and performing standing for layering to obtain a filtrate D. The method is simple to operate, mild in reaction condition, low in cost and high in product yield, and the purity and content of the obtained tildipirosin are both greater than 99%; and the method is beneficial to industrial production.