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Cefaclor preparation and preparation method thereof

A technology for cefaclor and preparations, applied in the field of medicine, can solve the problems of complicated purification and crystallization treatment, complicated reaction conditions, poor product quality and the like, and achieves the effects of fast reaction rate, high reaction yield and few by-products

Active Publication Date: 2016-07-20
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved in the present invention is to provide a cefaclor preparation and a preparation method thereof, so as to improve the product quality of the cefaclor preparation and improve the low conversion rate and poor product quality existing in the synthesis process of the existing cefaclor bulk drug , complex reaction conditions, complicated purification and crystallization treatment, etc.

Method used

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  • Cefaclor preparation and preparation method thereof
  • Cefaclor preparation and preparation method thereof
  • Cefaclor preparation and preparation method thereof

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preparation example Construction

[0046] The invention discloses a preparation method of cefaclor preparation, comprising the preparation of cefaclor crystals, pretreatment, weighing, mixing, molding and packaging of main materials and auxiliary materials, and the preparation of cefaclor crystals is based on 7-ACCA, Deng potassium Salt is used as a raw material, and cefaclor crystals are prepared through silanization reaction, acylation reaction, condensation reaction, acidolysis reaction, extraction and impurity removal, decolorization and crystallization steps.

[0047] The preparation method of cefaclor crystals in the present invention specifically comprises the following processing steps,

[0048] (1) Silanization reaction: Add 7-ACCA to dichloromethane, dissolve at a temperature of 25-30°C to obtain a 7-ACCA solution, add a silylating reagent to the 7-ACCA solution, and react at a temperature of 40-46 The silanization reaction is carried out at ℃, and the temperature is lowered to -15℃ after the reaction...

Embodiment 1

[0063] This embodiment is a preparation example of cefaclor crystals, using 7-ACCA and Deng potassium salt as raw materials, wherein: the content of 7-ACCA (HPLC) ≥ 98.0%, moisture ≤ 1.0%, and the content of Deng potassium salt ≥ 99%, moisture ≤0.5%.

[0064] The preparation of cefaclor crystals includes seven steps of silanization reaction, acylation reaction, condensation reaction, acidolysis reaction, extraction and removal of impurities, decolorization and crystallization.

[0065] 1.1 Silanization reaction

[0066] Add 40ml of dichloromethane solvent to the reactor, control the temperature at 25°C, accurately weigh 20.00g of 7-ACCA and add it into the reactor to obtain a 7-ACCA solution, control the temperature at 25°C, and add the complex silylating reagent , the composite silylating reagent includes 6.33g trimethylchlorosilane, 3.60g hexamethyldisilazane, 0.083g N, O-bistrimethylsilylacetamide, control the reaction temperature at 40°C, start the heating and reflux reac...

Embodiment 2

[0080] This example is a preparation example of cefaclor crystals, using 7-ACCA and Deng potassium salt as raw materials, wherein: adopting 7-ACCA and Deng potassium salt as raw materials, wherein: the content of 7-ACCA (HPLC)≥98.0% , Moisture ≤ 1.0%, Deng potassium salt content ≥ 99%, moisture ≤ 0.5%.

[0081] The preparation of cefaclor crystals includes seven steps of silanization reaction, acylation reaction, condensation reaction, acidolysis reaction, extraction and removal of impurities, decolorization and crystallization.

[0082] 1.1 Silanization reaction

[0083] Add 100ml of dichloromethane solvent to the reactor, control the temperature at 25°C, accurately weigh 20.00g of 7-ACCA and add it to the reactor to obtain a 7-ACCA solution, control the temperature at 30°C, and add the complex silylating reagent , the composite silylating reagent includes 10.00g trimethylchlorosilane, 9.40g hexamethyldisilazane, 0.200g N, O-bistrimethylsilylacetamide, control the reaction t...

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PUM

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Abstract

The invention discloses a cefaclor preparation and a preparation method thereof. The preparation method comprises: preparing cefaclor crystal, pretreating a main material and auxiliary materials, weighing, mixing, forming, and packaging; wherein the preparation of the cefaclor crystal includes subjecting 7-ACCA and potassium (R)-[(3-ethoxy-1-methyl-3-oxoprop-1-enyl)amino]phenylacetate to silylation, acylation, condensation, acid hydrolysis, extraction and cleaning, decoloring, and crystallization; the preparation comprises the cefaclor crystal as the main material and auxiliary materials, the cefaclor crystal is < / =33 degrees in angle of repose, 0.50-0.60 g / m in bulk density, 0.70-0.80 g / ml in compactness and 40-60 Mum in D10 of particle size distribution, 120-140 Mum in D50 and 210-230 Mum in D90. The conversion rate of cefaclor in chemical synthesis is increased, reaction conditions are simplified, the crystal form and particle size distribution of the cefaclor crystal are improved, and the quality of finished cefaclor crystal is improved.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a cefaclor preparation and a preparation method thereof. Background technique [0002] Cefaclor, chemical name: (6R,7R)-7-[(R)-2-amino-2-phenylacetamido]-3-chloro-8-oxo-5-thia-1- Azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid monohydrate. The chemical structural formula is shown below, [0003] [0004] Cefaclor is white to light yellow powder or crystalline powder; slightly odorous. Slightly soluble in water, almost insoluble in methanol, ethanol, chloroform or dichloromethane. [0005] Cefaclor is a β-lactam antibiotic, a cephalosporin drug, in the form of white to slightly yellow powder or crystalline powder; slightly odorous. It is a second-generation cephalosporin, which has the characteristics of strong effects of the first-generation cephalosporin on Gram-positive bacteria and the second-generation cephalosporin on Gram-negative bacteria. Penicillin-resistant Staphylo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K31/545C07D501/59C07D501/06C07D501/12A61P31/04
CPCA61K31/545C07B2200/13C07D501/06C07D501/12C07D501/59
Inventor 胡利敏张锁庆胡卫国杨梦德贾全张立斌柳世萍李敏张文胜魏宝军田洪年胡少华刘萍刘海席马亚松杜金松
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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