31 results about "Cefotetan Disodium" patented technology

The invention discloses cefotetan disodium and a preparation method of an intermediate of cefotetan disodium. Commercially-available raw materials, namely, 4-(1-amino-3-tert-butoxy-1,3-dioxo-2-alkenyl)-1,3-dithietane-2-carboxylic acid (2) and 7-MAC (3) are subjected to a condensation reaction to obtain a compound (4), and then the compound (4) is subjected to deprotection and salification to obtain cefotetan disodium (1). The invention further provides a preparation method of the compound (2). In the route, no chloride agent contaminating the environment in a conventional route is used, and the preparation method has the advantages of being simple in process route and environmentally friendly, lowering the process cost and increasing the total product yield and is suitable for industrial production.

The invention discloses a preparation method of high-purity cefotetan disodium for injection, which belongs to the field of production and purification process of cephalosporin antibiotics. The main raw materials are 7‑MAC, acylating agent and isothiazole monosodium salt. After the acylation reaction, hydrolysis reaction and condensation reaction, the active alumina chromatography column is used to purify and remove impurities, and then after steps such as decolorization, salt formation and refining, cefotetan disodium is finally obtained; the present invention can overcome organic solvents Residue and no quality risk caused by resin crushing, better product quality and lower impurity content, and lower cost, simple operation, energy saving and environmental protection, suitable for industrial production.

The invention discloses preparation of an impurity in cefetecol disodium and a structure confirmation method, and belongs to the pharmaceutical analysis technology field. Literature reports that a HPLC-MS method to carry out structure derivation of an impurity in a sample, but aimed to the impurity with a small content, satisfied results are difficult to obtain through the HPLC-MS method, and literature and patent reports related to the impurity are not discovered. Aimed to the above problem, separation is carried out by utilization of a preparation column, enrichment of the target impurity is carried out, further separation and purification are carried out, and finally the impurity monomer is obtained. Confirmation is carried out and the chemical structure of the impurity is obtained. The method is simple, the result is accurate, and the method can be used for impurity analysis control of cephalosporin samples.

The invention relates to a cephamycin intermediate compound and a preparation method thereof. The cephamycin intermediate compound has a structure of formula (I), and is prepared by directly reacting 7beta-chloroacetamide-7alpha-methoxy-3-(1-methyl-1H-tetrazole-5-thiomethyl)-3-cephem-4-carboxylic acid and dicyclohexylamine in a specific solvent to form a salt and crystallizing. The cephamycin intermediate compound has the characteristics of high purity, high stability and the like, is conductive to improving the purity of cephamycin final products such as cefminox sodium, cefmetazole sodium and cefotetan disodium, and is beneficial to large-scale production and application.

The invention discloses a preparation method of cefotetan disodium, which belongs to the technical field of medicine and comprises the following steps: A. Adding methanol into the reactor, stirring and controlling the temperature, then adding cefotetan acid, and then adding a salt-forming agent, stirring until dissolved to obtain a mixed solution; B. Control the temperature of the reactor, add a small amount of organic solvent until the system is slightly cloudy, and grow crystals once; C. After the first crystal growth is completed, add an organic solvent, carry out secondary crystal growth, and filter to obtain solid crystals of cefotetan disodium; D. The solid crystal of cefotetan disodium is washed, atomized and dried, and vacuum-dried to obtain the finished product of cefotetan disodium. The cefotetan disodium prepared by the invention has low impurity content, good fluidity, uniform particle size distribution, stable quality, easy subpackage of subsequent powder injection preparation products, and improved drug safety; the preparation method of the invention also has the advantages of simple operation , The advantages of energy saving and environmental protection.

The invention relates to a preparation method of cefmetazole. The preparation method comprises the steps of adopting a one-pot method containing 7-ACA, 1-methyl-5-tetrazole-thione and chloroacetyl chloride, obtaining 7-DCT, then using seven-position methoxy groups of sodium methylate and tert-butyl hypochlorite, and obtaining methoxy cephalosporin mother nuclei which are shared mother nuclei. The cefmetazole can serve as four methoxy cephalosporin products, namely cefminox, cefmetazole, cephalosporin and cefotetan disodium, three steps are omitted, the processing steps are greatly shortened, cost is lowered, and the overall yield is raised to 70%.

The invention discloses a novel crystal form of cefotetan acid, a method for preparing cefotetan disodium by the novel crystal form of the cefotetan acid and a pharmaceutical composition containing the cefotetan disodium. The X-ray diffraction pattern of the novel crystal form appears no X-ray diffraction peak; the endothermic peak in the differential thermal analysis pattern is positioned at 158.3 DEG C; the exothermic peak is positioned at 144.6 DEG C. The novel crystal form solves the technical problem of instability of the cefotetan disodium prepared by using the cefotetan acid in the prior art. The used preparation method has good operability and few residues of organic solvent, and is specifically suitable for large-scale industrial production.

The invention relates to the technical field of medicine and particularly relates to a preparation method for cefotetan disodium. In the preparation method, cefotetan acid is mixed with silica gel through a first salifying, then a first filter liquor is collected through a first filtering, the first filter liquor is mixed with EDTA and active carbon, a second filter liquor is collected through filtering, then acid-forming and crystallization are performed, and then cefotetan acid product is obtained through third filtration, collection and filter cake, as well as washing; and the cefotetan acid product is taken to be mixed with active carbon after second salifying, fourth filter liquor is collected through the fourth filtering, and then degerming and freeze drying are performed, namely the cefotetan disodium is obtained. The product prepared by using the method provided by the invention is white, is excellent in solution clarity after solution, is less in the variety of residual solvent, is low in content of relevant matters such as polymer and the like, the adopted process is simple, the raw materials are easy to access, and the method is suitable for large-scale industrial production.

The invention discloses a preparation method of an anti-infective cephalosporin drug. In the invention, compound III is prepared by reacting 7-MAC(II) with 2-oxoacetic acid hydrate, and compound III and 2-carbamoyl-3,3- Dimercaptoacrylic acid is subjected to acetalization reaction to prepare compound IV, and then cefotetan disodium (I) is obtained through deprotection and salt formation. The invention has simple synthesis route, mild reaction conditions, reduces the formation of impurities, improves the total yield and purity of products, and is suitable for industrial production.

The invention discloses a medicinal composition of cefotetan disodium, which comprises the cefotetan disodium, and also comprises minor ingredients; the percentage by mass of the cefotetan disodium is 50 to 99 percent; and the percentage by mass of the minor ingredients is 1 to 50 percent. The medicinal composition of the cefotetan disodium is added with the minor ingredients capable of strengthening the stability of the cefotetan disodium to inhibit the quick degradation of the cefotetan disodium when the cefotetan disodium meets water in the processes of production, storage and use and improve the stability of the cefotetan disodium, so that a high-efficiency and stable medicinal composition product of the cefotetan disodium is obtained.

The invention relates to a preparation method of a cephamycin intermediate. The cephamycin intermediate compound has a structure of formula (IV), and is prepared by reacting 7‑ACA with dichloroacetyl chloride in a specific solvent, reacting the obtained product with MMT under the catalysis of a sulfonic acid catalyst, and crystallizing. The cephamycin intermediate of the present invention has the characteristics of high purity and good stability, and is beneficial to improving the purity of cefamycin final products such as cefminox sodium, cefmetazole sodium and cefotetan disodium, and is beneficial to large-scale production and application .

The invention relates to a preparation method and a medicinal composition of a cefotetan disodium compound. The cefotetan disodium compound is crystal, wherein characteristic peak of the crystal in an X-ray powder diffraction pattern measured by using Cu-Ka ray is indicated in 2 theta of 8.0 degrees, 12.1 degrees, 15.4 degrees, 17.0 degrees, 19.8 degrees, 21.6 degrees, 23.0 degrees, 24.3 degrees, 25.7 degrees, 27.4 degrees, 30.7 degrees and 33.5 degrees. The compound crystal has good stability and hygroscopicity, and can be well stored and saved, so that the stability of cefotetan disodium is improved to a certain degree.