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Method for producing cephalothin acid by water phase method

A technology of cefotaxime acid and production method, applied in directions such as organic chemistry

Inactive Publication Date: 2011-05-04
湖南永利化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022]1) High production costs
Since the reaction, separation, and crystallization systems are all carried out in organic solvents, there are many types of organic solvents required (including halogenated alkanes, silylating reagents, acetone, ethyl acetate, petroleum ether, etc.), and the consumption is very large. The consumption is 20t / t or more, and the market prices of organic solvents are relatively high, thus greatly increasing production costs
[0023]2) High requirements for process operation and high labor intensity
[0024]3) There are many potential safety hazards and serious environmental pollution
During the production process, most of the systems are flammable, explosive, and volatile organic solvents. The production site has a strong odor, high safety requirements, and large environmental pollution.

Method used

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  • Method for producing cephalothin acid by water phase method
  • Method for producing cephalothin acid by water phase method
  • Method for producing cephalothin acid by water phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A production process for producing cefotaxime acid by an aqueous phase method. Its process flow chart is shown in Figure 1, and it is carried out according to the following steps in turn:

[0054] 1) React

[0055]At room temperature, add in sequence: deionized water 300L, 7-ACA 50Kg, organic solvent ethyl acetate 45L; then add about 40.0Kg of alkaline regulator sodium carbonate at room temperature within a certain period of time, and stir to 7- ACA dissolves completely. Cool the temperature of the system to about 10°C, and add about 20 L of 2-thiophene acetylation reagent 2-thiophene acetyl bromide within 150 min. After adding the material, time the reaction for 30 minutes. After the reaction is completed, add the reaction terminator sodium metabisulfite 5.0Kg , heat up to a certain temperature, add about 60.0Kg of sodium chloride, a precipitation accelerator, and let stand for 30 minutes to precipitate cefotaxime sodium; perform suction filtration at room temper...

Embodiment 2

[0064] A production technique for producing cefotaxime acid by an aqueous phase method is carried out successively according to the following steps:

[0065] At room temperature, add in sequence: 650L of deionized water, 100Kg of 7-ACA, and 100L of petroleum ether; then add about 85.0Kg of sodium bicarbonate at room temperature within a certain period of time, and stir until the 7-ACA is completely dissolved. Cool the temperature of the system to about 15 ℃, add about 45 L of 2-thiophene acetyl chloride within 120 min, after adding the material, time the reaction for 30 minutes, add 10.0Kg of sodium bisulfite after the reaction is completed, and add bromine at the temperature of 20 ℃. About 125.0Kg of sodium chloride, let stand for 30min to precipitate cefotaxime sodium; suction filtration at 10°C, and wash twice with petroleum ether totaling 165L to obtain cefotaxime sodium wet product.

Embodiment 3

[0067] The cefotaxime sodium wet product obtained in Example 2 was dissolved in 600 L of purified water at room temperature, 5.0 Kg of medical activated carbon was added, stirred for 30 min, suction filtered, and the filter and filter residue were washed with 120 L of purified water and 75 L of ethyl acetate, and collected. filtrate.

[0068] Collect the purified and decolorized filtrate, adjust the pH of the system to about 2.4-2.6 with hydrochloric acid at room temperature, stir and grow the crystals for 1 hour, cool and suction filtration, and wash the wet product with a total of 250L of purified water, take out the wet product and put it in the Vacuum dry at +42±2°C for 20-22 hours until H 2 O≤0.5%, about 64.0-68.0Kg of cefotaxime acid product is obtained.

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Abstract

The invention discloses a method for synthesizing cephalothin acid by using 7-aminocephalosporanic acid (7-ACA) as a raw material, which is characterized in that: the 7-ACA and a 2-thiophene acetylation reagent are subjected to condensation reaction in a water phase solvent, and the production process sequentially comprises the following steps of: performing condensation reaction on the 7-ACA in a water phase; performing centrifugal filtration on a reaction product; refining and decolorizing; and performing crystallization separation, centrifugal filtration and vacuum drying to obtain a cephalothin acid product. The production process is simplified, the requirement on equipment is reduced, the amount of an organic solvent can be saved by over 70 percent, potential safety hazard and environmental pollution due to high consumption of the inflammable, explosive and volatile organic solvent are eliminated, the safety requirement level of the production field is reduced, production cost is greatly reduced, and the method is easy to operate and suitable for mass production and has high technical and economic feasibility.

Description

technical field [0001] The invention relates to a preparation method of a cephalosporin pharmaceutical bulk drug, in particular to a production method of cephalothinic acid. Background technique [0002] Cephalothin, the chemical name is: (6R,7R)-3-[(acetoxy)methyl]-7-[2-(2-thienyl)acetamido]-8-oxo-5 -Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, its chemical structural formula (I) is as follows: [0003] [0004] (I) [0005] It is a synthetic semi-synthetic cefoxitin antibiotic—cefoxitin (English name: Cefoxitin, chemical name: (6R,7S)-3-carbamoyloxymethyl-7-methoxy-8-oxo- 7-[2-(2-thienyl)acetamido]-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid) (Ⅱ) main raw material, [0006] [0007] (II) [0008] The production of cephalothin acid both at home and abroad generally adopts the solvent method production process at present, and its process is as follows: [0009] 1), reaction [0010] Put 500L of purified water into the reaction kettle and coo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/06C07D501/04C07D501/12
Inventor 陆振荣刘志奇刘国定钟发敏梁杰李宁
Owner 湖南永利化工股份有限公司
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