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Preparation method of 3-deaminized formoxyl-cefuroxime acid crystal

A technology of cefuroxime acid and carbamoyl, which is applied in the field of preparation technology of 3-decarbamoyl-cefururoxime acid crystallization, which can solve problems such as filtration and drying difficulties, affecting product quality, and small particle size of the product, so as to shorten crystallization The effects of time, good fluidity, and low viscosity of crystal slurry

Inactive Publication Date: 2017-03-08
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no special crystallization method for its characteristics, resulting in long crystallization time, small product particle size, wide particle size distribution, high viscosity of crystal slurry, difficulty in filtration and drying, etc. in the production process, which affects the quality of the product, as well as the growth cycle and Cost of production

Method used

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  • Preparation method of 3-deaminized formoxyl-cefuroxime acid crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The 3-decarbamoyl-cefururoxime acid liquid prepared by the upstream synthesis process is used as raw material, wherein the content of 3-decarbamoyl-cefururoxime acid is 50 mg / mL, 280 mL is put into a 500 mL jacketed crystallizer, and the Circulating water bath keeps the temperature in the crystallizer at 2°C. Vacuumize the crystallizer with a vacuum pump to remove methylene chloride in the feed liquid. There are a lot of bubbles on the surface of the solution at the beginning, and stop degassing when there are no bubbles on the surface. Turn on stirring and adjust the rotation speed to 150r / min, slowly add dilute hydrochloric acid with a mass fraction of 10% to the crystallizer to adjust the pH value to 3.8, add 0.15g of treated seed crystals, change the stirring speed to 100r / min, and grow the crystal for 50min . Adjust the stirring to 110r / min, continue to slowly drop dilute hydrochloric acid into the crystallizer at a rate of 3mL / h to adjust the pH value to the end p...

Embodiment 2

[0030] The 3-decarbamoyl-cefururoxime acid liquid prepared by the upstream synthesis process is used as raw material, wherein the content of 3-decarbamoyl-cefururoxime acid is 50 mg / mL, 350 mL is put into a 500 mL jacketed crystallizer, and the Circulating water bath keeps the temperature in the crystallizer at 5°C. Use a vacuum pump to evacuate the crystallizer to remove methylene chloride in the feed liquid. There are a lot of bubbles on the surface of the solution at the beginning, and stop degassing when there are no bubbles on the surface. Turn on the stirring and adjust the rotation speed to 170r / min, slowly add dilute hydrochloric acid to the crystallizer to adjust the pH value to 3.7, add 0.15g of treated seed crystals, change the stirring speed to 100r / min, and grow the crystal for 45min. Adjust the stirring to 110r / min, continue to slowly drop dilute hydrochloric acid into the crystallizer at a rate of 4mL / h to adjust the pH value to the end point of 1.9, and grow the...

Embodiment 3

[0032] The 3-decarbamoyl-cefururoxime acid liquid prepared by the upstream synthesis process is used as raw material, wherein the content of 3-decarbamoyl-cefururoxime acid is 50 mg / mL, 350 mL is put into a 500 mL jacketed crystallizer, and the A circulating water bath kept the temperature inside the crystallizer at 4°C. Turn on the stirring and adjust the rotation speed to 160r / min, slowly add dilute hydrochloric acid to the crystallizer to adjust the pH value to 3.9, add 0.4g of the treated seed crystal, change the stirring speed to 100r / min, and grow the crystal for 45min. Adjust the stirring to 110r / min, continue to slowly drop dilute hydrochloric acid into the crystallizer at a rate of 3.9mL / h to adjust the pH value to the end point of 2.0, and grow crystals for 30min. Wash after filtering, soak and wash the crystals with 20mL of dichloromethane for 1min, filter; soak and wash the crystals with 120mL of cold purified water for 3 times, soak for 1min each time, and filter;...

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Abstract

The invention belongs to the technical field of a drug intermediate crystal, and particularly relates to a preparation method of 3-deaminized formoxyl-cefuroxime acid crystal. The raw material is 3- deaminized formoxyl-cefuroxime feed liquid prepared in an upstream synthesis process. The specific process includes steps of putting raw materials in a crystallizer according to matching ratio, removing methylene dichloride contained in the feed liquid, and maintaining constant temperature in the crystallizer; adjusting pH value by 10% of diluted hydrochloric acid by mass, and performing isoelectric point crystallization; before producing the crystal, adding the treated 3- deaminized formoxyl-cefuroxime crystal seed; after cultivating the crystal, adjusting pH value to the final point; performing secondary crystal cultivation, filtering, washing and drying, and obtaining a spherical 3-deaminized formoxyl-cefuroxime acid crystal product. The preparation process provided by the invention can effectively shorten the crystal time and avoid problems of too small product granularity and too wide granularity distribution in the production of the 3-deaminized formoxyl-cefuroxime acid; furthermore, the filtering and drying performances are improved, and the production capacity of the production line is promoted.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical intermediate crystallization, and in particular relates to a preparation process for 3-decarbamoyl-cefuroxim acid crystallization. Background technique [0002] 3-Decarbamoyl-cefuroxime acid, English name: 3-to carbamoyl-cefuroxime acid, CAS number: 56271-94-4, molecular formula: C 15 h 15 N 3 o 7 S, relative molecular mass 381.361, density 1.72g / cm 3 , is a white crystalline powder, odorless and tasteless, insoluble in water and dichloromethane, and is an intermediate for the preparation of cefuroxime. The structural formula is as follows: [0003] [0004] Cefuroxime has the characteristics of broad-spectrum antibacterial effect and low nephrotoxicity. The drug binds to the penicillin-binding protein on the bacterial cell membrane, inhibits cell division and growth, and finally dissolves and dies the bacteria. Therefore, it is widely used to combat sensitive Various infections cau...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/12
CPCC07D501/34C07D501/12
Inventor 孙华刘宝树栗晓特宋梦燕
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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