- Novel production process of ceftiofur
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The invention discloses a preparation method of a novel production process of ceftiofur. The method comprises the following steps of: synthesizing 7-amino- 3-[(2-furyl-carbonyl)-thiomethyl]-3-cephem-4-carboxylic acid; adding the 7-amino- 3-[(2-furyl-carbonyl)-thiomethyl]-3-cephem-4-carboxylic acid into dichloromethane, and performing stirring; slowly dropwise adding triethylamine, and performing stirring; slowly adding AE-active ester, then adding water, and performing stirring; performing still standing for layering, and separating out a water phase; adding purified water into an organic phase, performing stirring, separating out a water phase, combining the water phases, washing with dichloromethane, adding activated carbon into the water phase for decoloration, and performing suction filtration; adjusting the pH value of a filtrate to 2.5, and carrying out suction filtration; dissolving a filter cake with acetone, adding activated carbon for decolorization, and filtering out the activated carbon; and slowly dropwise adding water into an acetone solution, and performing crystallizing, filtering, washing and drying to obtain ceftiofur. The purification method is simple, short in production period, low in cost and beneficial to industrial large-scale production; gas with high difficulty and toxicity is not used, and therefore, production difficulty is low, and the cost is low.
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Paragraph 0016
(2021/01/30)
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- Preparation method of ceftiofur intermediate
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The invention relates to a preparation method of a ceftiofur intermediate. According to the method, hydroxymethyl-7-aminocephalosporanic acid and thiocarbamide are reacted with each other, so as to obtain mercaptomethyl-7-aminocephalosporanic acid, the mercaptomethyl-7-aminocephalosporanic acid and furoyl chloride are fed into different solvents and organic alkali is added in a refining conditionor a non-refining condition, decoloration is performed through esterification, and pH adjustment processing is performed, so as to obtain the ceftiofur intermediate. The method is not involved in severe reaction conditions and special production equipment, adopted materials and reagents are cheap, easy to get, and low in toxicity, obtained products are high in purity, high in yield and low in cost, and the method is easy to operate and easy for industrial production.
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Paragraph 0014; 0034; 0037; 0038; 0042-0043; 0047-0048
(2018/10/27)
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- Method for synthesizing ceftiofur intermediate and ceftiofur
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The invention belongs to the technical field of chemical synthesis, and concretely relates to a method for synthesizing a cefotaxime intermediate 7-amino-3-[(2-furyl-carbonyl)-thiomethyl]-3-cephem-4-carboxylic acid and ceftiofur. The method comprises the following steps: sequentially adding 7-aminocephalosporanic acid, thiofurancarboxylic acid, a solid base catalyst gamma-Al2O2-O2Na, zeolite and water into a reaction kettle, performing stirring and reacting at room temperature for 1.5-2.5 h, filtering the obtained reaction solution, adjusting the pH value of the obtained filtrate to 5.5-6.5 by using an appropriate amount of hydrochloric acid, filtering the filtrate, washing the obtained filter cake with water to obtain a white solid, and performing vacuum drying to obtain the 7-amino-3-[(2-furyl-carbonyl)-thiomethyl]-3-cephem-4-carboxylic acid. The method uses water as a solvent, so the production cost is reduced, the produced products have a high yield and a high purity, and the promotion of industrial production is benefited.
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Paragraph 0024; 0025; 0026
(2019/01/07)
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