76639-93-5Relevant articles and documents
Method for synthesis of florfenicol
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, (2017/08/27)
The invention discloses a method for synthesis of florfenicol and belongs to the technical field of medicine synthesis. 1-R1-2-(R)-4- methylsulfino phenyl formyl aziridine is dissolved in solvent to react with sterically hindered reductant to form chiral alkamine compound 1 with a single configuration; compound 1 is heated and reacts with triethylamine hydrofluoride in the solvent to form (1R, 2S)-3-fluoride-1-4-(methylsulfino phenyl)-2-(R1-amido)-1-propyl alcohol; (1R, 2S)-3-fluoride-1-4-(methylsulfino phenyl)-2-(R1-amido)-1-propyl alcohol has the blocking group taken away in the solvent to form (1R 2S)-2-amido-3-fluoride-1-4-methylsulfino phenyl-1-propyl alcohol; florfenicol can then be obtained through dichloro-acetylation reaction of (1R, 2S)-2-amido-3-fluoride-1-4-methylsulfino phenyl-1-propyl alcohol.
FLORFENICOL SYNTHESIZING METHOD
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Paragraph 0120; 0121, (2016/11/17)
The present invention discloses a new florfenicol synthesizing method. The method synthesizes florfenicol products meeting requirements of the Drug Administration by a series of combinations of cyclization, selective reduction, fluorinated open ring, deprotection and acylation, hydroxyl sulfoacid esterified configuration converting reaction, hydrolysis reaction and the like. The synthesizing method of the present invention utilizing chiral amine closed-ring aziridine three-membered ring uses a physical separation method to repeatedly purify chiral aminoketone of high yield obtaining single R configuration, and uses selective reduction and converts the configuration to obtain florfenicol, greatly improving atom economy, while avoiding waste water pollution caused by the existing process, and greatly reducing costs for treating waste water and reducing pollution to the environment, thus lowering costs and simplifying the process. In addition, the present invention uses triethylamine hydrofluoride as a fluorinated open-ring reagent, to improve safety of a liquid reaction compared to a gas reaction and reduce corrosion of equipment, facilitating industrial production.
A substituted 1,2-aminoalcohols method for preparation of drug
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, (2016/10/07)
The invention discloses a preparation method of a substituted 1, 2-alkamine medicine. The preparation method comprises the following steps: dissolving a compound A into a solvent, then adding alkali, stirring, dripping a carbonylation agent, and after dripping, stirring, so as to obtain a compound B; dissolving the compound B into the solvent, adding a reducing agent, controlling the temperature of a reaction liquid to range from 10 DEG C below zero to 50 DEG C, and stirring, so as to obtain a compound C; adding the compound C into the solvent, using Ishikawa agent for fluoridation, after fluoridation, obtaining a compound D, removing the solvent, directly adding into acid for hydrolysis so as to obtain a compound E; resolving the compound E, ester and alkali into the solvent for reaction for 2 to 24 hours under a temperature of 0 to 50 DEG C, so as to obtain a compound F; the process route has the characteristics of short production period, low cost and high yield, the operation is simple and convenient, the product yield is increased while unit operation is shortened, and the preparation method is suitable for industrial production.