Preparation method of thiamphenicol

Abstract

The invention relates to a preparation method of antibiotic, in particular to a preparation method of thiamphenicol. The preparation method comprises the following steps: by weight, dissolving 100 parts of D-4-Methylsulfonylphenyl serine ethyl ester in 500-700 parts of methanol solvent, adding 24-27 parts of KBH4 to react at 30-60 DEG C for 4-8 hours, recycling 300-400 parts of methanol, neutralizing reaction solution with acid to adjust the pH value of the solution to 6-10, adding 42-45 parts of dichloroacetonitrile, performing a cyclization reaction for 4-6 hours, reducing pressure to recycle all of the solution, adding water to perform solid-liquid separation and obtain a solid mixture, adding 600-800 parts of water in the solid mixture, heating to 85-90 DEG C, keeping temperature at 85-90 DEG C for 30 minutes, and discoloring to obtain thiamphenicol. The invention is characterized by fewer steps, simple operation, short reaction time, low cost and the like.

Description

technical field The invention relates to a preparation method of antibiotics, in particular to a preparation method of thiamphenicol. Background technique Thiamphenicol is an antibiotic, mainly used for various infectious diseases caused by sensitive bacteria, and is generally produced by synthetic methods. US: 3927054 uses p-thiamphenicol benzaldehyde to produce thiamphenicol through condensation, esterification, resolution, reductive acylation, acidification, etc., which has the disadvantages of long process route, low yield, many wastes, and high production cost; CN101200441A Using D-threo-2-(dichloromethyl)-4,5-dihydro-5-[p-(thymphenyl)phenyl]-4-oxazolemethanol (III) to prepare thiamphenicol element, but the process of purifying raw materials is complex and wastes a large amount of isomer D--threo-2-(dichloromethyl)-4,5-dihydro-a-[p-(thymphenyl)phenyl] -4-oxazole methanol (IV), resulting in low yield, high cost, long reaction time and other shortcomings. Contents of ...

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Problems solved by technology

US: 3927054 uses p-thiamphenicol benzaldehyde to produce thiamphenicol through condensation, esterification, resolution, reductive acylation, acidification, etc., which has the disadvantages of long process route, low yield, many wastes, and high production cost; CN101200441A Using D-threo-2-(dichloromethyl)-4,5-dihydro-5-[p-(thymphenyl)phenyl]-4-oxazolemethanol (III) to prepare thiamphenicol element, but the process of purifying raw materials is complex and wastes a large amount of isomer D--threo-2-(dichloromethyl)-4,5-dihydro-a-[p-(thymphenyl)phenyl] -4-oxazole methanol (IV), resulting in low yield, high cost, long reaction time and other shortcomings

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