A kind of cefotiam hydrochloride drying process

A technology of cefotiam hydrochloride and drying process, which is applied in the direction of drying gas arrangement, partial agitation dryer, static material dryer, etc. It can solve the problems of difficulty in reducing production costs, difficulty in reaching pharmacopoeia limits, high moisture content in products, etc. problems, to achieve the effect of simple operation, easy control of reaction temperature, high overall yield and purity

Active Publication Date: 2020-05-22
SHANDONG LUOXIN PHARMA GRP CO LTD +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The total yield of the product is low, and the total yield of the preparation reported in the literature is about 20%, which makes it difficult to reduce the production cost
[0006] 2. There are many by-products, more than 2% of the standard stipulated in the Japanese Pharmacopoeia
[0007] 3. The product obtained by crystallization has high humidity and high moisture content. It is difficult to remove it by conventional drying methods, and it is difficult to reach the limit specified in the Pharmacopoeia.

Method used

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  • A kind of cefotiam hydrochloride drying process

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Embodiment 1

[0030] 1. Preparation of refined wet product of cefotiam hydrochloride:

[0031] a. 17.32kg (100mol) of 1-(2-dimethylaminoethyl)-1,2,3,4-tetrazole-5-thiol (DMMT), boron trifluoride-acetonitrile (250mol, according to BF 3 ), acetonitrile 100L, and butanol 50L were added to the reaction tank, and the temperature was controlled at 0-5°C, and 27.23kg (100mol) of 7-ACA was slowly added dropwise, controlled at 0-5°C and stirred for 1.5h. During the reaction, 200mol of 2M hydrochloric acid, after the reaction was completed, ethanol was added for crystallization, centrifuged, and double-cone drying to obtain 35.75kg of intermediate 1 with a yield of 92% and a purity of 99.2%;

[0032] B, 15.33kg (100mol) of phosphorus oxychloride, 80L acetonitrile, 20L N, N-dimethylformamide, 150mol triethylamine are dropped into reaction tank, then drop into aminothiazole acetic acid hydrochloride 19.46kg (100mol), Stirring reaction was carried out at -5~-10°C for 1 hour. After the reaction was com...

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Abstract

The invention discloses a drying process of cefotian hydrochloride, and belongs to the technical field of medicine. The drying process comprises the following steps: a purified wet product of cefotianhydrochloride is transferred into a drying device, and the moisture in the wet product is removed by adopted hot air, thereby meeting the requirements of industrial production. The drying device provided by the invention mainly comprises a filter, a flow sensor, a temperature sensor, a pressure sensor, a heat exchanger and a solenoid valve. The drying process and the drying device provided by theinvention can improve the yield and the purity of the product and control the moisture content below 3%, and are suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of medicines, in particular to a cefotiam hydrochloride drying process. Background technique [0002] Cefotiam hydrochloride is a second-generation antibiotic for injection, and its dihydrochloride and buffer sodium carbonate mixed powder preparation (trade name Pansporin) is clinically used. The effect of this product on Gram-positive bacteria is similar to that of cefazolin, and it has a strong antibacterial effect on Escherichia coli, Klebsiella pneumoniae, Proteus mirabilis, and Haemophilus. [0003] It also has antibacterial effect on Citrobacter, Enterobacter, and indole-positive proteus. [0004] In the existing method for preparing cefotiam axetil hydrochloride, there are following deficiencies: [0005] 1. The total yield of the product is low, and the total yield of the preparation reported in the literature is about 20%, which makes it difficult to reduce the production cost. [0006] 2. There ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/06C07D501/36F26B9/06F26B21/10F26B21/12
CPCC07D501/06C07D501/36F26B9/06F26B21/001F26B21/10F26B21/12
Inventor 刘庆利李兆文窦成金
Owner SHANDONG LUOXIN PHARMA GRP CO LTD
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