Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Cefminox sodium compound crystal, preparation method of cefminox sodium compound crystal and sterile powder injection containing cefminox sodium compound crystal

A technology of cefminox sodium and sterile powder injection, which is applied in the fields of medical preparations containing active ingredients, organic chemistry, powder delivery, etc., and can solve problems such as threats to patient safety and anaphylactic shock reactions of cefminox sodium

Active Publication Date: 2012-12-26
HAINAN HERUI PHARMA
View PDF7 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] However, like other drugs of the same class, cefminox sodium often causes anaphylactic shock reactions in clinical practice, which seriously threatens the safety of patients.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Cefminox sodium compound crystal, preparation method of cefminox sodium compound crystal and sterile powder injection containing cefminox sodium compound crystal
  • Cefminox sodium compound crystal, preparation method of cefminox sodium compound crystal and sterile powder injection containing cefminox sodium compound crystal
  • Cefminox sodium compound crystal, preparation method of cefminox sodium compound crystal and sterile powder injection containing cefminox sodium compound crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] [Example 1] Prepare cefminox sodium heptahydrate with reference to prior art

[0062] The cefminox sodium raw material is prepared according to the method of Example 4 of the US4357331 manual, and 92g of 7β-bromoacetamido-7α-methoxyl-3-(1-methyl-1H-tetrazol-5-yl)sulfur) Methyl)-3-cephalosporin-4-carboxylic acid was suspended in 1L of water, and saturated aqueous sodium bicarbonate solution was added to adjust its pH to 7.2 at low temperature, and 46.3g of D-cysteine ​​salt was added to the mixed solution salt, cooled, and stirred at room temperature for 30 to 40 minutes, during which time the pH was adjusted to between 7.1 and 7.2. The reaction mixture was subjected to column separation using a 50 x 700 cm column (containing 8000 ml of Diaion HP-20), washed with water, and 52.6 g of cefminox sodium were obtained from the water-eluted fraction.

[0063] Cefminox sodium heptahydrate is prepared according to the method of US4555404 specification example 1, 10.3 g of cefmi...

Embodiment 2

[0066] [embodiment 2] the preparation of cefminox sodium compound crystal

[0067] Under room temperature conditions, drop into 5g cefminox sodium heptahydrate crude product to reactor, add the water dissolving of 50ml, stir 28 minutes, filter, regulate filtrate pH with glacial acetic acid and be 6.3, the temperature of control filtrate is 18 ℃, in every At a stirring speed of 100 rpm, slowly add 200ml of a mixed solution of absolute ethanol and acetone (the volume ratio of absolute ethanol and acetone is 1:3) dropwise at a speed of 420ml / h until the crystals are precipitated, and then at 30 Under constant stirring, control the supersaturated concentration of the solution, continue to slowly add 200ml of n-butanol and tetrahydrofuran mixed solution (the volume ratio of n-butanol and tetrahydrofuran is 2:1), make the crystallization complete, filter, and use 50ml of absolute ethanol and acetone The mixed solution was washed twice, sucked dry, and dried under reduced pressure to...

Embodiment 3

[0070] [embodiment 3] the preparation of cefminox sodium compound crystal

[0071] Under room temperature conditions, drop into 5g cefminox sodium heptahydrate crude product to reactor, add the water dissolving of 50ml, stir 28 minutes, filter, regulate filtrate pH with glacial acetic acid and be 6.9, the temperature of control filtrate is 30 ℃, in every At a stirring speed of 150 revolutions per minute, slowly add 200ml of a mixed solution of absolute ethanol and acetone (the volume ratio of absolute ethanol and acetone is 1:8) dropwise at a speed of 480ml / h until the crystals are precipitated, and then at 70 per minute Under constant stirring, control the supersaturated concentration of the solution, continue to slowly add 600ml of n-butanol and tetrahydrofuran mixed solution (the volume ratio of n-butanol and tetrahydrofuran is 5:1), make the crystallization complete, filter, and use 50ml of absolute ethanol and acetone The mixed solution was washed twice, sucked dry, and d...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to a cefminox sodium compound crystal, a preparation method of the cefminox sodium compound crystal and a sterile powder injection containing the cefminox sodium compound crystal. The cefminox sodium compound crystal is provided with an X-ray diffraction pattern as shown in a picture 3. The cefminox sodium compound crystal is a novel crystal form different from cefminox sodium heptahydrate reported in literatures, and tests prove that the cefminox sodium compound crystal in the crystal form has low content of a high-molecular polymer and excellent stability; in addition, the content of the high-molecular polymer slightly increases as the storage time prolongs.

Description

technical field [0001] The invention belongs to the field of preparation of pharmaceutical compounds, and in particular relates to a cefminox sodium compound crystal, a preparation method thereof, and a sterile powder injection containing the compound crystal. Background technique [0002] Cefminox sodium, English name: Cefminox Sodium, its chemical name is: (6R,7S)-7-[[[[(S)-2-(2-amino-2-carboxyethyl)mercapto]acetamide ]-7-methoxy-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[ 4.2.0] Oct-2-ene-2-carboxylic acid sodium salt, molecular formula: C 16 h 20 N 7 o 7 S 3 Na, molecular weight: 541.57, chemical structural formula is the following formula (I): [0003] [0004] Formula (I) [0005] Cefminox sodium is a third-generation cephalosporin antibiotic, which has good antibacterial effect on Gram-negative and positive, especially Escherichia coli, Klebsiella, Haemophilus influenzae, Proteus and fragilis Bacteroides have a strong antibacteria...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/57C07D501/12A61K31/546A61K9/14A61P31/04
Inventor 朱正兵张金花
Owner HAINAN HERUI PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com