Process for synthesizing clindamycin phosphate

A technology of clindamycin phosphate and synthesis process, which is applied in the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., can solve the problems of high pressure, high pyridine price and high production cost, and achieves simple process method and high yield rate, the effect of reducing the pressure of discharge

Inactive Publication Date: 2010-11-24
ZHANGJIAGANG XINYI CHEM
View PDF1 Cites 12 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The above process scheme has the following disadvantages: (1) use a large amount of pyridine (or pyridine and triethylamine), because pyridine is expensive, so the production cost is very high...

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 3.4-Synthesis of Clindamycin Condensate (Protect)

[0015] (1) Take 40Kg, 150Kg, and 25Kg of clindamycin hydrochloride alcoholate, acetone, and phosphorus oxychloride respectively, mix the above three substances, and react with heat preservation and stirring for 4 hours at -10~20°C;

[0016] (2) Take respectively 60Kg and 500Kg of sodium carbonate and water, mix and dissolve, then add it to the product obtained in step (1), stir and crystallize, and centrifuge to obtain 3.4-clindamycin condensate (protectant) wet Taste;

[0017] (3) Dried product obtained by drying: 35.5Kg, weight yield 88.75%.

Embodiment 2

[0019] 3.4-Synthesis of Clindamycin Condensate (Protect)

[0020] (1) Take 80Kg, 250Kg, and 50Kg of clindamycin hydrochloride alcoholate, acetone, and phosphorus oxychloride respectively, mix the above three substances, and heat and stir for 6 hours at -10~20°C;

[0021] (2) Take 100Kg and 1000Kg of sodium carbonate and water respectively, mix and dissolve, then add it to the product obtained in step (1), stir and crystallize, and centrifuge to obtain 3.4-clindamycin condensate (protected product) wet Taste.

[0022] (3) Dried product obtained by drying: 72.5Kg, weight yield 90.63%.

Embodiment 3

[0024] Synthesis of Clindamycin Phosphate

[0025] (1) Get respectively 40Kg, 240Kg, 50Kg, 30Kg, 5Kg, 5Kg of the 3.4-clindamycin condensate (protection) obtained in Example 1 and acetone, phosphorus oxychloride, salt of wormwood, DMAP, TEBA-C1 , mix the above-mentioned substances, and keep warm for 8 hours at -10-20°C;

[0026] (2) Add 2000Kg of water to the product obtained in step (1), and keep it warm for 4 hours at -10 to 20°C;

[0027] (3) Adsorption and crystallization: the product obtained in step (2) is subjected to adsorption, crystallization, and centrifugation to obtain a wet product of clindamycin phosphate according to conventional methods.

[0028] (4) Dried product obtained by drying: 39.1Kg, weight yield 97.75%.

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

No PUM Login to view more

Abstract

The invention relates to a process for synthesizing clindamycin phosphate. The process comprises the following steps: 1) ketal reaction, wherein clindamycin hydrochloride alcoholate is used as a basic raw material to prepare a 3.4-clindamycin condensation compound through selective hydroxyl protection; and 2) phosphatidic reaction, wherein the 3.4-clindamycin condensation compound is used as a raw material, phosphorus oxychloride is used as a phosphatidic agent, and anhydrous potassium carbonate is used as an acid binding agent to complete the phosphatidic reaction under double actions of esterification catalyst dimethylamino pyridine and phase-transfer catalyst benzyl triethyl ammonium chloride, and a target compound, namely the clindamycin phosphate, can be obtained through hydrolysis deprotection. The process has the advantages that: 1, the process has simple method and practical application; 2, the content of pyridine/triethylamine in wastewater of phosphatidic reacting process can be controlled, so that the pressure of high COD wastewater drainage can be greatly reduced; and 3, the weight yield reaches over 95 percent, and the product quality fulfills the requirement of WS1-(X-322)-2003Z.

Description

technical field [0001] The invention relates to a new synthesis technique of clindamycin phosphate. Background technique [0002] As a broad-spectrum antibiotic raw material, clindamycin phosphate is widely used clinically. It is a semi-synthetic derivative of lincomycin, and its mechanism of action is to inhibit bacterial protein synthesis. The antibacterial spectrum of this product is the same as that of lincomycin, and it is effective against Gram-positive bacteria such as Staphylococcus aureus, Staphylococcus epidermidis, Streptococcus hemolyticus, Streptococcus viridans, Pneumococcus pneumoniae, and Bacillus diphtheria, as well as Peptococcus, Peptostreptococcus, Anaerobic bacteria such as Bacteroides fragilis, Fusobacterium, Eubacterium, and Propionibacterium have antibacterial effects. At present, the commonly used synthetic technique of clindamycin phosphate is: use 3.4-clindamycin condensate (protectant) as raw material, use phosphorus oxychloride as phosphating ag...

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
IPC IPC(8): C07H15/16C07H1/02
Inventor 楼新灿陈立坤
Owner ZHANGJIAGANG XINYI CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap