5575-21-3Relevant academic research and scientific papers
Synthesizing and purifying method of cefalonium
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Paragraph 0018; 0020; 0023; 0024, (2018/01/09)
The invention discloses a synthesizing and purifying method of cefalonium and belongs to the technical field of medicine production. The method comprises a synthesizing step and a purifying step, wherein the synthesizing step comprises a synthesizing step of a cefalonium intermediate and a synthesizing step of a cefalonium coarse product. The method is characterized by comprising the step of obtaining a cefalonium fine product through the purifying step by means of the synthesizing step of the cefalonium intermediate and the synthesizing step of the cefalonium coarse product by taking D-7ACA as a raw material. The method disclosed by the invention has the beneficial effects that the process is slow in reaction and relatively high in safety; by introducing a catalyst, the reaction time is shortened greatly, and the production efficiency is increased; and the production cost is lowered greatly by successfully replacing 7-ACA by D-7ACA.
A method for preparing cephalosporin Loening
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Paragraph 0036; 0041; 0046; 0051; 0056, (2017/08/26)
The invention relates to a preparation method of cefalonium. According to the preparation method, raw materials (cefalotin and pyrazinamide) react at a low temperature to obtain the product cefalonium. The preparation method particularly comprises the following steps: dissolving cefalotin acid into an organic acid, carrying out carboxyl protection by using a silanization protection reagent and then carrying out iodination reaction on reaction products and iodotrimethylsilane; then carrying out amination reaction on the reaction product from the former step and pyrazinamide; and finally carrying out deprotection by alcoholysis, regulating the pH value at a low temperature and crystalizing to obtain cefalonium. According to the preparation method of cefalonium, cefalotin acid is protected by the silanization protection reagent in an organic solvent and then reacts with iodotrimethylsilane; the reaction time is short, the reaction conditions are mild, the reaction is complete and no side reaction is almost generated; due to adoption of a mixed solvent crystallization method, the characteristics of high drying speed, light color and high yield can be achieved; in addition, the used solvent can be recycled and the amount of generated sewage can be reduced; therefore, the preparation method of cefalonium has remarkable economic and environmental benefits and facilitates industrial production.
A 7-amino cephalosporanic acid one-step process for preparing method for the preparation of cephalosporin Loening
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Paragraph 0032-0040, (2017/02/09)
The invention discloses a method for preparing cephalonium from 7-aminocephalosporanic acid at one step. The method comprises the following steps: (1) adding 7-aminocephalosporanic acid into water with the temperature of 0-10 DEG C; (2) regulating the pH value of the solution; (3) adding an organic solvent, tiophencacetyl chloride and ethyl acetate, and reacting for 1-3h while stirring at the temperature of 0-10 DEG C; (4) after the reaction is ended, standing for layering; (5) adding activated carbon into a water phase for decoloring, and carrying out suction filtration; (6) adjusting the pH value of the filtrate, then, adding isonicotinamide, and reacting at the temperature of 15-50 DEG C; (7) after the reaction is ended, growing the grain for over 1h; (8) filtering to obtain a crystal, and drying to obtain the cephalonium. The cephalonium is prepared at one step, and an intermediate is not needed to be separated and extracted in the reaction process, so that the method is simple and convenient in operation, simple in reaction step and high in yield; the 7-aminocephalosporanic acid is used as the raw material and is simple and easy to obtain and low in market price, so that the production cost is greatly reduced.
