11 results about "Sitafloxacin" patented technology

The invention provides a preparation method of sitafloxacin intermediate 5-benzyl-7 (S)-tertiary butyl carbonyl amino-5-azaspiro [2, 4] heptane, which comprises the following steps: carrying out condensation reaction on 5-benzyl-4, 7-dioxo-5-azaspiro [2, 4] heptane serving as an initial raw material and (S)-tertiary butyl sulfinamide to obtain imine, reducing the imine and reducing amide under the action of a reducing agent to obtain 5-benzyl-7 (S)-tertiary butyl carbonyl amino-5-azaspiro [2, 4] heptane. And removing tert-butyl sulfinyl from the obtained reduction product under an acidic condition, and finally, carrying out protection by tert-butyloxycarboryl to obtain the 5-benzyl-7 (S)-tert-butyl carbonyl amino-5-azaspiro [2, 4] heptane. The synthesis method provided by the invention is simple and convenient to operate, mild in reaction condition, relatively short in production period, good in stereoselectivity and more suitable for industrial production, and the obtained product has high yield and optical purity.

The invention relates to the technical field of pharmaceutical preparations. Specifically, the invention relates to a sitafloxacin tablet and a preparation method thereof. The sitafloxacin tablet comprises (1) a solid dispersion which comprises (a) an active component which is sitafloxacin sesquihydrate and accounts for 15%-30% of the total weight of the tablet, (b) a solid dispersion carrier which is copovidone and accounts for 45%-65% of the total weight of the tablet, and (c) a stabilizer which is colloidal silicon dioxide and accounts for 0.1%-2.2% of the total weight of the tablet; (2) a filler accounting for 10-40% of the total weight of the tablet; (3) an adhesive accounting for 1%-5% of the total weight of the tablet; (4) a disintegrating agent accounting for 0.5-3% of the total weight of the tablet; and (5) a lubricant accounting for 0.2%-1.0% of the total weight of the tablet.

This invention provides a compound, its preparation method, and its application, as well as a method for preparing a five-membered ring intermediate of sitafloxacin, relating to the field of chemical drug preparation technology. The compound provided by this invention has the structure shown in Formula 1. In this invention, the compound shown in Formula 1 is a novel intermediate. Using it to prepare the five-membered ring intermediate of sitafloxacin (Formula 3) requires no Pd / C and hydrogenation process, and does not form a five-membered ring-opening impurity (Formula 6). The process is simple and suitable for industrial production. This invention provides a method for preparing the five-membered ring intermediate of sitafloxacin (structure shown in Formula 3). In the embodiments of this invention, the prepared five-membered ring intermediate of sitafloxacin with the structure shown in Formula 3 was analyzed by HPLC, and no ring-opening impurity as shown in Formula 6 was detected, with a high yield. Formula 1.

The invention relates to the technical field of injection filling, and particularly discloses filling equipment for preventing sitafloxacin injection from being degraded, the filling equipment comprises an equipment base and a filling container, the filling container is located at the top of the equipment base, the upper surface of the equipment base is fixedly connected with a supporting seat, and the upper surface of the supporting seat is fixedly connected with a supporting platform; the upper surface of the supporting platform is fixedly connected with a discharging barrel, the upper surface of the discharging barrel is fixedly connected with a motor, and the inner side of the supporting base is provided with a feeding assembly used for achieving stable circulating feeding of the filling containers; according to the cisastasacin injection filling device, cisastasacin injection can be filled into the filling container in a sealed mode through the filling pipe, contact between the injection and the external environment is reduced, external microorganisms, dust, impurities and the like are effectively prevented from entering the injection, the pollution risk is reduced, meanwhile, the oxidation speed, the degradation speed and the microorganism breeding speed are reduced, and therefore the purity and quality of the injection are guaranteed; and the storage life of the injection is prolonged.

The application relates to the field of drug synthesis, and particularly discloses a high-efficiency asymmetric synthesis method of a sitafloxacin intermediate (1S, 2S)-2-fluorocyclopropane carboxylic acid, which comprises the following steps: S1. reacting a compound SM1 with a chiral compound SM2 in a solvent under the action of an alkali to obtain an epoxide ring-opening chiral compound 1; S2. introducing a group into a hydroxyl group in the compound 1 to obtain a compound 2; S3. obtaining an absolute chiral configuration cyclopropane compound 3 from the compound 2 under the action of an alkali; S4. obtaining an absolute chiral configuration compound 4 from the compound 3 after a deprotection group; S5. generating an absolute chiral configuration compound 5 by oxidizing the compound 4 with an oxidizing agent; and S5. removing a benzene (sulfo) sulfonyl group from the compound 5 to obtain the absolute chiral configuration (1S, 2S)-2-fluorocyclopropane carboxylic acid. The preparation method has the advantages that starting materials are easy to obtain, each step in the synthesis process is simple in operation and separation and extraction, the reaction conditions are mild, the cis-trans selectivity is special, the enantioselectivity is high, the total yield and production capacity are high, and the method is suitable for large-scale industrial production.

This invention relates to a method for synthesizing the sitafloxacin intermediate 5-benzyl-7(S)-tert-butoxycarbonylamino-5-azaspiro[2,4]heptane. The method uses 1-benzylmethylpyrrolidine-2,4-dione as the starting material and proceeds through five steps: cyclization, oxime formation, chiral asymmetric reduction, salt formation, and amino protection to obtain the target product. Specifically, the cyclization reaction uses an alkylating agent and a base to construct a spirocyclic structure; the oxime reaction introduces a methoxyimino group via methoxyamine hydrochloride; the chiral asymmetric reduction uses a catalytic system composed of a chiral ligand and a boron reagent to construct the chiral center, followed by purification via maleic acid salt formation; and finally, the amino group is protected with di-tert-butyl dicarbonate to obtain the target product. This invention offers high atom economy, good process scalability, simple operation, controllable cost, and high product purity, providing a reliable intermediate synthesis scheme for the efficient preparation of sitafloxacin active pharmaceutical ingredient.

The application provides a sitafloxacin intermediate and an enzymatic preparation method and application thereof, and belongs to the technical field of organic synthesis and enzyme catalysis. The sitafloxacin intermediate compound 3 is a key chiral intermediate for preparing sitafloxacin. The preparation method comprises the following steps: (1) reacting compound 1 with an azide reagent to obtain compound 2; (2) catalyzing and reacting compound 2 by using a transaminase to obtain compound 3. The preparation method for preparing compound TM by using compound 3 comprises the following steps: (A) reducing compound 3 by using a reducing reagent and carrying out amine-ester exchange to obtain compound 4; (B) reacting compound 4 with a Boc reagent to obtain compound 5; (C) reducing compound 5 to obtain product TM. The process is simple in operation, conventional reaction equipment is used, raw materials are cheap and easy to obtain, the yield is high, the process introduces the biological enzyme catalysis technology, high stereoselectivity product is obtained, and the cost is greatly reduced.

The present invention relates to the technical field of pharmaceutical preparations. Specifically, the present invention relates to a sitafloxacin tablet and a preparation method thereof. The sitafloxacin tablet comprises: (1) a solid dispersion, wherein the solid dispersion comprises: (a) an active ingredient, which is sitafloxacin sesquihydrate, accounting for 15%-30% of the total weight of the tablet, (b) a solid dispersion carrier, wherein the solid dispersion carrier is copovidone, accounting for 45%-65% of the total weight of the tablet, (c) a stabilizer, wherein the stabilizer is colloidal silicon dioxide, accounting for 0.1%-2.2% of the total weight of the tablet; (2) a filler, accounting for 10%-40% of the total weight of the tablet; (3) a binder, accounting for 1%-5% of the total weight of the tablet; (4) a disintegrant, accounting for 0.5%-3% of the total weight of the tablet; and (5) a lubricant, accounting for 0.2%-1.0% of the total weight of the tablet.

The invention relates to the technical field of pharmaceutical preparations, in particular to a preparation method of a coating solution of a sitafloxacin coated tablet, and when the sitafloxacin coated tablet is prepared by the method disclosed by the invention, the rapid disintegration of the tablet is not influenced while relatively high coating weight gain is ensured.

The invention relates to the technical field of chemical medicine preparation, and discloses stable sitafloxacin intermediate processing equipment which comprises a box body, a bottom shell is fixedly connected to the bottom of the inner wall of the box body, and a cooling mechanism used for separating out a sitafloxacin intermediate from a solution is arranged in the bottom shell. A mixing mechanism for fully mixing a sitafloxacin intermediate solution is arranged at the top of the box body and comprises a motor, the motor is fixedly connected to the top of the box body, a threaded column is fixedly connected to an output shaft of the motor, and a limiting pipe is fixedly connected to the top wall of an inner cavity of the box body; the sitafloxacin intermediate solution in the container is cooled through the second heat conduction pipe, so that the sitafloxacin intermediate in the solution is crystallized and separated out, the stirring rod is still in a continuous rotating state in the process, heat in the solution is evenly distributed, local overheating or supercooling is avoided, crystals are dispersed in the solution, the agglomeration phenomenon is prevented, and the stability of the sitafloxacin intermediate solution is improved. Therefore, the uniformity and the quality of crystallization are improved.

The invention belongs to the field of chemical drug synthesis, and particularly relates to a preparation method of an antibacterial drug sitafloxacin intermediate. The preparation method comprises the following steps: carrying out condensation reaction on a compound I and N, N-dimethylformamide dimethyl acetal to prepare an intermediate IV; the intermediate IV and (1R, 2S)-1-amino-2-fluorocyclopropane are subjected to a substitution reaction, and an antibacterial drug sitafloxacin intermediate compound III is prepared. The preparation method disclosed by the invention has the advantages of mild reaction conditions, short reaction time, small and single solvent dosage, high reaction conversion rate and high selectivity, and meets the requirements of industrial large-scale production.