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Method for recovery of cefaclor

A technology of cefaclor and recovery method, which is applied in the field of recovery of cefaclor, can solve problems such as not involving transformation, achieve the effect of reducing losses, simple recovery method, and easy operation

Inactive Publication Date: 2006-09-13
苏州盛达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the patent WO9931109, cefaclor was synthesized by enzymatic method, and cefaclor was separated from the reaction system with 1-naphthol and 2-naphthol, but it did not involve the synthesis of cefaclor from cefaclor 1-naphthol complex and the method converted from cefaclor 2-naphthol complex

Method used

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  • Method for recovery of cefaclor

Examples

Experimental program
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Effect test

Embodiment 1

[0033] In the 10000ml reaction bottle, add cefaclor content and be 6000ml of cefaclor aqueous solution of 14.78g / l, under stirring, add 80g pulverized 1-naphthol (particle size is less than 100 μm) at room temperature, adjust the solution so that the pH of the solution is 4-5, stir at room temperature for 1-2 hours, then cool down to 0-5°C, stir and react for 2-3 hours, filter, wash with appropriate amount of water and acetone, and vacuum-dry at 30-35°C to obtain light yellow cefaclor complex 137.1g (80.87% dry content). The residual cefaclor in the aqueous solution of cefaclor was 1.02 g / l, and the recovery rate was about 95%.

[0034] Add 100 g of the prepared cefaclor complex in portions to a mixed solution of 100 ml of water and 500 ml of N, N-dimethylformamide or N, N-dimethylacetamide, keep the temperature at 10-20 ° C, and use Adjust the pH to 1.5-2.0 with concentrated hydrochloric acid to dissolve, filter, wash with 50ml N,N-dimethylformamide or N,N-dimethylacetamide,...

Embodiment 2

[0037] In a 10000ml reaction bottle, add 6000ml of cefaclor aqueous solution with cefaclor content of 14.78g / l, under stirring, add 85g of pulverized 2-naphthol (particle size is less than 100μm) at room temperature, adjust the pH to 4~5, and stir at room temperature 1 to 2 hours, then lower the temperature to 0 to 5°C, stir and react for 2 to 3 hours, filter, wash with appropriate amount of water and acetone, and dry in vacuum at 30 to 35°C to obtain 121.5g of light yellow cefaclor complex (dried content was 80.46%). The cefaclor aqueous solution contained 2.35 g / l of cefaclor, and the recovery rate was about 84%.

[0038]Add 100 g of the prepared cefaclor complex into 100 ml of water and 500 ml of N,N-dimethylformyl or N,N-dimethylacetamide mixed solution in portions, keep the temperature at 10-20°C, and use concentrated Adjust the pH to 1.5-2.0 with hydrochloric acid to dissolve, filter, wash with 50ml N,N-dimethylformamide or N,N-dimethylacetamide, combine the filtrate an...

Embodiment 3

[0041] In a 1000ml reaction flask, add 200ml of cefaclor aqueous solution with a cefaclor content of 14.78g / l, cool down to 0-10°C under stirring, add 600ml of N,N-dimethylformamide or N,N-dimethylformamide Methyl acetamide, adjust the pH to 6-7, keep at 20-28°C, stir for 1 hour, cool down to 5-10°C, stir for 1-2 hours, filter, wash with an appropriate amount of ethyl acetate, and vacuum-dry at 30-35°C to obtain white Cefaclor N, N-dimethylformamide complex or cefaclor N, N-dimethylacetamide complex is about 3.51 g (74.17% on a dry basis). The residual cefaclor in the mother liquor was 1.47g / l, and the recovery rate was about 87%.

[0042] Then the obtained cefaclor N, N-dimethylformamide complex or cefaclor N, N-dimethylacetamide complex is dissolved in water under the condition of adding acid, and the pH value is adjusted with alkali After making it crystallized, the solid and liquid are separated, and then washed with a washing solvent to obtain crystallized cefaclor hydra...

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Abstract

The invention discloses a recovering technique of reclaiming the cefaclor from the water liquor. Firstly, the cefaclor in the water liquor is transformed into the cefaclor composite; secondly, the cefaclor composite is transformed into the cefaclor N, N-dimethylformamide composite or the cefaclor N, N-dimethyl acetamide composite, finally, the cefaclor N, N- dimethylformamide or the cefaclor N, N-dimethyl acetamide composite is transformed into the cefaclor hydrate to reclaim the cefaclor. Comparing the invention with the existing technique, we can perorate that the invention can reclaim the height ratio of the cefaclor from the cefaclor equeous solution and is easy to operating.

Description

technical field [0001] The invention relates to a method for recovering cefaclor, in particular to a method for recovering cefaclor from an aqueous solution of cefaclor. Background technique [0002] Cefaclor is a semi-synthetic second-generation β-lactam antibiotic, which has strong antibacterial activity against Gram-positive bacteria, high efficiency, broad-spectrum, and good chemical stability. one of the important drugs. [0003] The chemical structural formula of cefaclor sees I: [0004] [0005] x=1,2 [0006] I [0007] Since cefaclor was successfully marketed in the 1970s, it has been highly praised by people for its high efficiency, broad spectrum and good clinical safety. In the known synthetic methods of cefaclor (such as: US5608055; US5693790; WO9931109), the cefaclor finished products are prepared by reaction crystallization in an aqueous solution. Because cefaclor has certain solubility in water, its solubility is about 2...

Claims

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Application Information

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IPC IPC(8): C07D501/12C07D501/59
Inventor 方长明
Owner 苏州盛达药业有限公司
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