- Synthesis method of cefprozil
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The invention discloses a synthesis method of cefprozil. The method comprises the following steps: carrying out a reaction of a compound II and di-tert-butyl dicarbonate ester under the condition of 4-dimethylaminopyridine to prepare a compound III, after reaction between the compound III and oxalyl chloride, carrying out a reaction between the compound III and a compound IV to prepare a compoundV, and performing deprotection to prepare the final product, namely cefprozil (I). The raw materials for the reaction are easily available, the process route is simple, the total yield is high, the byproducts are few and the method is suitable for industrialized production.
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Paragraph 0011; 0042-0050
(2020/06/24)
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- Preparation method of cefprozil
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The invention relates to a preparation method of cefprozil. A synthesis method comprises the following steps: taking 7-ACA (7-aminocephalosporanic acid) as a starting raw material; after carrying outsilylation protection, carrying out a series of reactions including iodination and the like to generate a compound 2; taking the compound 2 to react with methyl D-(-)-4-hydroxy-phenylglycinate under the catalysis of immobilized penicillin acylase to generate a compound 1, so as to obtain a target product cefprozil. The preparation method provided by the invention has the advantages of moderate reaction conditions, environmental friendliness, high conversion ratio, simple technology and high cis-isomer content.
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Paragraph 0024-0031; 0036-0041
(2019/04/14)
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- Preparation method of cefprozil
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The invention relates to the technical field of preparation of antibiotics, and specifically discloses a preparation method of cefprozil. The preparation method is characterized by taking GCLE (7-phenylacetyl amino-3-chloromethyl-3-cephem-4-carboxylic acid p-methoxybenzyl ester) as a starting material, and carrying out hydroformylation, ethylation and dewatering, thus obtaining GPRE; then hydrolyzing, thus obtaining APRA; firstly protecting hydroxyl groups and amino groups of p-hydroxyl phenylglycine, then carrying out condensation reaction with the APRA, and then deprotecting, thus obtainingthe cefprozil. According to the preparation method disclosed by the invention, toxic triphenyl phosphine is not used for preparing phosphine salt, so that the method is more environment-friendly; a reaction route requires no wittig reaction, so that the cost is lower; the hydroxyl groups and the amino groups of the p-hydroxyl phenylglycine are protected by adopting chloromethyl methyl ether and then are in reacting with a compound as shown in a formula VI, the cost is low, a deprotection reaction system is neutral, and the yield and the purity of a product are favorably increased.
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Paragraph 0023; 0024; 0025; 0026; 0027-0031
(2019/02/04)
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- Cefprozil refining method
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The invention discloses a cefprozil refining method. The method includes: (1) dissolving a crude cefprozil product in a mixed solvent of deionized water, ethanol and dichloromethane, conducting heating reflux dissolution to prepare a saturated or supersaturated solution; (2) performing cooling to 20-30DEG C, adding activated carbon for decolorization, conducting filtration, cooling the filtrate to5DEG C-10DEG C, performing crystallization for 1h, conducting cooling to 0DEG C-5DEG C, and performing crystal growing; (3) conducting filtering, and performing leaching with ethanol to obtain a white solid; and (4) placing the white solid obtained by step (3) in a vacuum drying box, conducting vacuum pumping, and performing drying for 3h or more, thus obtaining cefprozil crystals. The refining method provided by the invention remarkably improves the product quality, and is simple in operation, thus being suitable for industrial production.
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Paragraph 0027-0028; 0031-0035; 0038-0042; 0045-0047
(2019/12/02)
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