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Chloramphenicol sodium succinate synthesis method
Active Publication Date: 2019-07-19
ZHENGZHOU MINGZE MEDICAL TECH
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Problems solved by technology
[0005] The technical problem addressed by the present invention is: in the prior art, most of the techniques for preparing chloramphenicol succinate have defects such as large loss of raw materials, incomplete purification, and low purity; Process reports, very few records have directly prepared the finished product of sodium chloramphenicol succinate
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preparation example Construction
[0047] The invention provides a kind of synthetic method of sodium succinate chloramphenicol, comprising the following steps:
[0048] (1) At first, chloramphenicol and succinic anhydride are used as raw materials to react in the presence of a solvent and a catalyst. After the reaction is completed, the reaction solution is subjected to rotary evaporation, and then dissolved, washed, dried, and rotary evaporated to obtain amber Crude chloramphenicol acid;
[0049] (2) With the chloramphenicol succinate crude product obtained in step (1) and ethanolamine as raw materials, react in a solvent, after the reaction is completed, the reaction solution obtained is left to stand for crystallization and suction filtration at room temperature to obtain amber Chloramphenicol crude product;
[0050] (3) the ammonium succinate chloramphenicol obtained in step (2) is refluxed in anhydrousmethanol for beating, and suction filtered to obtain the chloramphenicol ammonium succinate white powde...
Embodiment example
[0052] The invention provides an implementation case of a sodium succinate chloramphenicol synthetic method, and the method may further comprise the steps:
[0053] (1) Preparation of chloramphenicol succinate crude product
[0054] A: Dissolve chloramphenicol in a solvent and mix evenly, then add catalyst and succinic anhydride (solid) sequentially at 0-30°C, and react at constant temperature for 3.5-6 hours after complete addition. After the reaction is completed, adjust the pH of the solution The value is 6-7, and then the solvent is removed by rotary evaporation at 30-40°C to obtain a viscous oil;
[0055] B: Add ethyl acetate to the viscous oily substance obtained in step A to dissolve, then wash and separate the solution, collect the organic phase, dry the organic phase, and remove the solvent by rotary evaporation at 30-40°C. Obtain viscous chloramphenicol succinate crude product;
[0056] In this process, a sufficient amount of ethyl acetate is used to fully dissolve...
Embodiment 1
[0087] A kind of synthetic method of sodium chloramphenicol succinate, the method comprises the following steps:
[0088] (1) Preparation of sodium chloramphenicol crude product
[0089] First add 3.6L tetrahydrofuran in the dry flask, slowly add 600g chloramphenicol therein under stirring, after the chloramphenicol is completely dissolved, add 80ml pyridine, cool to 0 ℃ after pyridine adds completely, then add 279g succinic anhydride (butane Add dianhydride in three batches, after the catalyst is completely added, start adding succinic anhydride, add one batch every half an hour), after succinic anhydride is added completely, react at 0°C for 4 to 5 hours; after the reaction is completed, use Quench the reaction with 4mol / L hydrochloric acid, adjust the pH of the solution to 6-7; then spin off the tetrahydrofuran at 40°C to viscous oil (no liquid drips out);
[0090] The obtained viscous oil was placed in 1.2L of ethyl acetate and stirred until it was completely dissolved, t...
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Abstract
The invention discloses a chloramphenicolsodium succinate synthesis method, which comprises: preparing chloramphenicol hemisuccinate by using chloramphenicol and succinic anhydride as raw materials,preparing chloramphenicol succinamide from the chloramphenicol hemisuccinate and ethanolamine, carrying out acidification treatment on the chloramphenicol succinamide to obtain high-purity chloramphenicol hemisuccinate monoester, and preparing chloramphenicol sodium succinate by using the chloramphenicol hemisuccinate monoester and sodium isooctanoate as raw materials. According to the present invention, the chloramphenicol sodium succinate is directly prepared by using the simple and easily-available preparation process, and has characteristics of high purity and high yield; the obtained product can be directly used so as to simplify the use process and achieve the good use effect; and the synthesis method provides the reliable method for the industrial preparation of chloramphenicol sodium succinate, has advantages of easily available raw materials, mild reaction conditions, short time, solventrecovery, simple and easy-performing operation, simple equipment and the like, and has theproduct yield of over 80%, wherein the content determined by liquid chromatography and UV-visible spectrophotometer is up to more than 99%.
Description
technical field [0001] The invention belongs to the technical field of medicine synthesis. Specifically relate to a kind of synthetic method of sodium chloramphenicol succinate. Background technique [0002] Chloramphenicol is an antibiotic produced by Streptomyces venezuela. It is a broad-spectrum antibiotic that can produce antibacterial effects by inhibiting bacterial protein synthesis. It is effective against most Gram-negative and positive bacteria, especially typhoid and paratyphoid bacillus It has the strongest effect; it also has a strong effect on influenza bacillus, pertussis bacillus, and Shigella, and it also has inhibitory effects on Escherichia coli, pneumonia bacillus, Proteus, and Pseudomonas aeruginosa. [0003] However, chloramphenicol has strong toxicity to bone marrow, and direct use will cause greater harm to the human body. Therefore, the research on the relationship between the structural modification and activity of chloramphenicol has attracted wid...
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