A kind of preparation technology of 7-atca

A 7-ATCA and preparation technology, applied in the direction of organic chemistry, etc., can solve problems such as unstable product performance, high cost, backward raw material preparation process, etc., and achieve the effect of solving color difference, increasing content, and improving work efficiency

Active Publication Date: 2017-11-07
HENAN KANGDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the expansion of the market, large-scale production of products has disadvantages such as backward raw materials and preparation technology, high cost, and unstable product performance. Only by reducing costs and improving product stability can we remain invincible in the competition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation process for 7-ATCA, comprising the following steps:

[0027] (1) After mixing 200g of dimethyl carbonate and 140g of boron trifluoride dimethyl carbonate complex, add 100g of 7-ACA and 45g of mercaptotetrazolium successively, stir and react at 15-20°C, and pass through the liquid phase When detecting 7-ACA residue ≤ 1%, the reaction is considered complete;

[0028] (2) Lower the reaction solution to 5-15°C, add 300g of purified water at 5-15°C, BF 3 Hydrolysis; the hydrolysis temperature is 5-15°C, and the hydrolysis time is 20-22 minutes;

[0029] (3) After adding 500g of dichloromethane for one extraction, add 250g of dichloromethane to the water layer for secondary extraction;

[0030] (4) Add ammonia water dropwise to the water intake layer at 0-10°C until the pH is 3.4-3.6. During the dropping process, control the temperature not to exceed 10°C. After the drop is complete, stir and grow crystals at 0-10°C for 2 hours;

[0031] (5) Centrifuge, wash ...

Embodiment 2

[0033] A preparation process for 7-ATCA, comprising the following steps:

[0034] (1) After mixing 200g of dimethyl carbonate and 200g of boron trifluoride dimethyl carbonate complex, add 100g of 7-ACA and 46g of methylmercaptotetrazolium successively, stir and react at 15-20°C, and pass through the liquid phase When detecting 7-ACA residue ≤ 1%, the reaction is considered complete;

[0035] (2) Lower the reaction solution to 5-15°C, add 300g of purified water at 5-15°C, BF 3 Hydrolysis; the hydrolysis temperature is 5-15°C, and the hydrolysis time is 20-22 minutes;

[0036] (3) After adding 600g of dichloromethane for one extraction, add 300g of dichloromethane to the water layer for secondary extraction;

[0037] (4) Add ammonia water dropwise to the water intake layer at 0-10°C until the pH is 3.4-3.6. During the dropping process, control the temperature not to exceed 10°C. After the drop is complete, stir and grow crystals at 0-10°C for 2 hours;

[0038] (5) Centrifuge,...

Embodiment 3

[0040] A preparation process for 7-ATCA, comprising the following steps:

[0041] (1) After mixing 250g of dimethyl carbonate and 200g of boron trifluoride dimethyl carbonate complex, add 100g of 7-ACA and 48g of mercaptotetrazolium successively, stir and react at 15-20°C, and pass through the liquid phase When detecting 7-ACA residue ≤ 1%, the reaction is considered complete;

[0042] (2) Lower the reaction solution to 5-15°C, add 350g of purified water at 5-15°C, BF 3 Hydrolysis; the hydrolysis temperature is 5-15°C, and the hydrolysis time is 20-22 minutes;

[0043] (3) After adding 650g of dichloromethane for one extraction, add 350g of dichloromethane to the water layer for secondary extraction;

[0044] (4) Add ammonia water dropwise to the water intake layer at 0-10°C until the pH is 3.4-3.6. During the dropping process, control the temperature not to exceed 10°C. After the drop is complete, stir and grow crystals at 0-10°C for 2 hours;

[0045] (5) Centrifuge, wash ...

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PUM

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Abstract

The invention relates to a preparation process of 7-ATCA. The preparation process comprises the following steps: (1) mixing dimethyl carbonate with a boron trifluoride dimethyl carbonate complex, adding 7-ACA and methimazole tetrazolylazo, and stirring to react at 15-20 DEG C until the residue of 7-ACA is less than or equal to 1% by virtue of liquid detection; (2) cooling reaction liquid to 5-15 DEG C, and adding purified water with the temperature of 5-15 DEG C for hydrolysis; (3) after adding dichloromethane for once extraction, adding dichloromethane into a water layer for secondary extraction; (4) dropwise adding weak base into the water layer at 0-10 DEG C until the pH is 3.4-3.6, and stirring to grow crystals at 0-10 DEG C for 2h, wherein the temperature in the dropwise adding process does not exceed 10 DEG C; and (5) carrying out centrifugation, sequentially washing with purified water and acetone, and drying, so as to obtain 7-ATCA. By virtue of the preparation process, a 7-ATCA product with good crystal form and particle size can be obtained and is a white crystal, the purity can reach 99.5% or above, and the mass yield can reach 115% or above.

Description

technical field [0001] The invention belongs to the technical field of preparation of pharmaceutical compounds, and in particular relates to a preparation process of 7-ATCA. Background technique [0002] 7-ATCA is also known as 7-TMCA, 7-ACT (tetrazolium ring), 3-(1-methyl-1-H-tetrazol-5-yl)thiomethyl 7-aminocephalosporanic acid. This is a relatively commonly used cephalosporin chemical pharmaceutical intermediate, such as cephalosporins cefoperazone sodium, cefminox, cefmetazole, cefpiramide, etc. are synthesized with 7-ATCA as the parent and then introduced different side chains . The quality of 7-ATCA products will directly affect key quality index parameters such as color grade, content, single impurity, and total impurity of the final product, so 7-ATCA is the key to the quality of such cephalosporin antibiotics. [0003] Moreover, with my country's accession to the WTO, the country's requirements for drug quality are increasing day by day, and at the same time, the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/24C07D501/04
CPCC07D501/04C07D501/24
Inventor 李文杰高德瀛李志军孙津鸽刘红坤韩新正李红德
Owner HENAN KANGDA PHARMA
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