328898-40-4Relevant articles and documents
Synthesis and purification method of tildipirosin
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, (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.
20,23-dihalogenation-5-O-mycarose amino-tylolactone and synthesizing method and application thereof
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, (2018/07/30)
The invention discloses 20,23-dihalogenation-5-O-mycarose amino-tylolactone and a synthesizing method and application thereof. The structural formula of 20,23-dihalogenation-5-O-mycarose amino-tylolactone is shown in the description. The preparing method of 1, 20,23-dihalogenation-5-O-mycarose amino-tylolactone comprises the steps of under nitrogen protection, dissolving and placing tylosin phosphate into an ice-water bath reaction container, adding reductant under stirring, and after conducting a stirring reaction for 3-24 hours, stopping nitrogen protection to obtain a mixed product; 2, adding an acid solution into a reaction container containing the mixed product until the pH value of a system is 1-2, conducting hydrolysis at 45-50 DEG C for 1-24 hours to obtain an intermediate coarse product, and after refining, obtaining a white solid intermediate; 3, at minus 5-0 DEG C, dissolving the intermediate into dichloromethane, adding triphenylphosphine, catalyst and halogenating agent under stirring, after adding, continuing the reaction at low temperature of minus 5-0 DEG C for 1-8 hours to obtain a coarse product, and after refining, obtaining 20,23-dihalogenation-5-O-mycarose amino-tylolactone. 20,23-dihalogenation-5-O-mycarose amino-tylolactone is a novel intermediate for synthesizing tildipirosin and can be used for synthesizing tildipirosin. The synthesizing method is simple in reaction path and convenient to operate, and the synthesizing cost is lowered by a large margin.
Preparation method of tildipirosin
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, (2017/08/29)
The invention provides a preparation method of tildipirosin. The preparation method comprises the following steps: tylosin A is hydrolyzed in an acidic solution, a hydrolysis product is extracted into an organic solvent A after hydrolysis, a sulfonate esterification reagent is added for sulfonate acidification reaction in the presence of alkali, extraction and layering are performed after the reaction, and a sulfonate esterified product is prepared; finally, the sulfonate esterified product is dissolved in an organic solvent B, piperidine and formic acid are added for a reductive amination reaction, a solvent is removed by distillation after the reaction, then an organic solvent C is added to dissolve the remaining reaction product, piperidine and alkali are added for an ammoniation reaction, acid is added after the reaction for extraction, layering and alkali regulation, and the final product of tildipirosin is prepared. The preparation method has the advantages that the reaction route is shortened, the total yield is increased, the reaction condition is mild, the operation is simple, and industrial production is facilitated.