Method for preparing tardocillin

A technology of benzathine penicillin and dibenzylethylenediamine is applied in the production and preparation field of benzathine penicillin, and can solve the problems of increased manufacturing cost, small crystal particle size, difficult control of reaction speed, etc., and achieves improved yield, reduced toxicity, The effect of improving product quality and safety

Active Publication Date: 2011-02-16
NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above-mentioned first kind of synthetic technique, its used solvent is nontoxic and harmless, but this method has the disadvantages that the reaction speed is difficult to control, the crystal particle size of the product is small, the loss when carrying out solid-liquid separation and washing and refining is large, and the product yield is low; Two kinds of synthetic techniques, although the yield of product, purity are improved relatively, and product particle size is controlled, but its effect is still not ideal enough
In particular, the controllable range of product granularity is narrow, and it is difficult to meet the needs of users for various granularities.
In order to solve this problem, the effective control of product particle size can only be achieved by increasing the amount of methanol or repeated grinding.
This greatly increases the manufacturing cost of the product
Furthermore, since methanol is a toxic solvent, the residual methanol in the final product not only has potential adverse effects on patients, but also causes great harm to operators and the ecological environment in the production process.

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
  • Method for preparing tardocillin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] At room temperature, add 40g of DBED to 350ml of ethanol with an alcohol concentration of 66% to make solution A; add 81g of penicillin G potassium to 1000ml of ethanol with an alcohol concentration of 66% to make solution B, and adjust the pH value of the solution to 6.2-6.8 . Start stirring and adjust it to 100r / min, add 4.5ml of A solution to B solution in advance, and continue to add the remaining A solution to B solution at a speed of 5L1 / min to obtain a suspension of benzathine penicillin, after suction filtration The filter cake was washed twice with 200ml of water and 95% ethyl acetate solution, and vacuum-dried for 120 minutes to obtain benzathine penicillin dry powder with a particle size of 100%≤80 μm.

Embodiment 2

[0026] At room temperature, add 50Kg DBED to 340L of 60% ethanol, press it into the DBED metering tank through pre-filtration and sterilizing filtration; Sterilize and filter and press into the crystallization tank. Start stirring and adjust it to 150r / min, add 3.6L of DBED solution to the crystallization tank in advance, and add the remaining DBED solution to the penicillin G sodium solution at a speed of 10L / min to obtain a suspension of sterile benzathine penicillin liquid, the filter cake obtained by suction filtration was washed twice with 200L water for injection and 150L 95% ethyl acetate solution, and dried in vacuum for 240 minutes to obtain sterile benzathine penicillin dry powder, which was mixed to obtain sterile benzathine penicillin powder, and then packed to obtain the finished product , particle size 100% ≤ 60μm.

example example 3

[0028] At room temperature, add 40Kg DBED to 50% ethanol to adjust to 400L, and press it into the DBED metering tank through pre-filtration and sterilizing filtration; Filtration and sterile filtration are pressed into the crystallization tank. Start the stirring and adjust it to 200r / min, add 3.2L of DBED solution in advance to the crystallization tank, and continue to add the remaining DBED solution to the penicillin G potassium solution at a speed of 15L / min to obtain a mixture of sterile benzathine penicillin. Suspension, the filter cake obtained by suction filtration was washed twice with 200L water for injection and 150L 95% ethyl acetate respectively, and vacuum-dried for 240 minutes to obtain sterile benzathine penicillin dry powder, which was subpackaged to obtain finished products with a particle size of 100%≤30 μm.

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
particle sizeaaaaaaaaaa
Login to view more

Abstract

The invention discloses a preparing method of benzathine penicillin which comprises the following procedures: a, 50 percent to 75 percent of ethanol is added to a raw medicine of the N, N-dibenzyl ethylenediamine diacetate, and is prepared into solvent A; b, 50 percent to 75 percent of ethanol is added to the raw medicine of penicillin G salt, and is prepared into solvent B; c, the pre-applied solvent A is added to the solvent B for stirring, then the residual solvent A is added to the solvent B, thus obtaining nzathine benzylpenicillin suspension; d, filtering and then washing and drying arecarried out on the nzathine benzylpenicillin suspension. The method has the advantages of improving yield coefficient of products, purity quotient and the controllability of particle size, reducing the toxicity of the residual solvent, improving the quality and safety of products and avoiding the harm of methanol to environment and human body at the same time.

Description

technical field [0001] The invention relates to a production and preparation method of pharmaceutical raw materials, in particular to a production and preparation method of benzathine penicillin. Background technique [0002] Benzathine penicillin, also known as long-acting penicillin, its English name is BenzathineBenzylpenicillin, its chemical name is (2S, 5R, 6R)-3,3-dimethyl-6-(2-phenylacetamido)-7-oxo-4 -Thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid N,N / -dibenzyldiethylamine salt tetrahydrate. In 1950, the United States patent (US2627491) disclosed the synthesis method of this compound for the first time. There are two kinds of processing routes for producing benzathine penicillin at present, and a kind of is the synthetic processing route of using water as solvent, is about to add N,N-dibenzylethylenediamine diacetate (hereinafter referred to as DBED) into appropriate amount of water and be mixed with solution A , Add penicillin G sodium to an appropriate amount ...

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 Patents(China)
IPC IPC(8): C07D499/60C07D499/14
Inventor 李晓宇张义恩刘树林郝小良何东召杨志方郭俊赵俭韩志伟张立荣夏学军高任龙王卫兵
Owner NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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