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Ganciclovir purification process

A technology of ganciclovir and process, which is applied in the field of refining process of ganciclovir, can solve the problems of increasing product production cost, poor product quality, unreachable, etc., and achieve cost saving, less crystallization times, reduction of waste and environmental protection pollution effect

Active Publication Date: 2010-10-06
SHANGHAI YIWEI INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ganciclovir is a multi-step chemical reaction, and some process intermediate steps involve isomer resolution, so the yield is low-cost and high. The domestic process mainly uses 2,9-diacetylguanine as the starting material, and 1, 3-dichloromethoxyl-2-propoxymethanol acetate carries out condensation reaction, carries out esterolysis reaction with acetic anhydride again, hydrolyzes and refines to obtain Ganciclovir crude product, finally four crystallization refines just can reach Pharmacopoeia standard again, but Unable to meet the requirements of the United States Pharmacopoeia for related substances, which also restricts the export of this product. Therefore, finding a refining process for ganciclovir can not only improve the quality of drug use for Chinese people, enhance drug safety, but also generate considerable income for the export of this product. economic benefits
At present, simply dissolving in an aqueous solution to crystallize and refine, the quality of the obtained product is very poor, and it must be recrystallized many times, which also causes a lot of waste and increases the production cost of the product. Therefore, finding an efficient refining method will greatly reduce the cost. The production cost of ciclovir can also reduce waste and environmental pollution in the production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] When producing ganciclovir, after the preliminary treatment of the synthetic product, the available content is 95%, and 10 kilograms of ganciclovir crude product of maximum impurity 4.8%, first adding concentration is 20 liters of sodium hydroxide solution of 7%, heat up 35 ℃, stirring and slowly adding a mass concentration of 7% sodium hydroxide solution until the material liquid is substantially clear, a total of 37 liters of 7% sodium hydroxide solution was added, then 2 kilograms of gac was added, and the temperature was stirred for 2 hours. Filter to obtain a clarified filtrate, raise the temperature of the filtrate to 50°C, and add ethanol dropwise at a rate of 70 liters / hour. Crystals appear in the feed liquid, and when it becomes turbid, stop adding ethanol, continue adding ethanol after half an hour, and add 222% ethanol in total. After adding ethanol, slowly lower the temperature to 15°C, filter to obtain the wet product of ganciclovir sodium salt, the content ...

Embodiment 2

[0023] When producing ganciclovir, after the initial treatment of the synthesized product, the available content is 96%, the maximum impurity is 3.7%, and 20 kg of crude product is added. 40 liters of 7% sodium hydroxide solution is added, the temperature is raised to 35 ° C, stirred and slowly added 7% sodium hydroxide solution, until the material liquid is substantially clear, add 75 liters of 7% sodium hydroxide solution altogether, then add 4 kilograms of gac, keep stirring for 2 hours, filter to obtain clarified filtrate, and the temperature of the filtrate is raised to 50 ° C. Add ethanol dropwise at a rate of 130 liters / hour. When crystals appear in the feed solution and become turbid, stop adding ethanol and continue adding ethanol after half an hour. Add 450 liters of ethanol in total. Slowly cool down to 15°C after adding ethanol, and filter to obtain Ganciclovir sodium salt wet product, content 99.2%, the largest impurity is 0.6%; Dissolve ganciclovir sodium salt in ...

Embodiment 3

[0025] A refinement process of ganciclovir is that the crude product of ganciclovir is basified by an alkaline solution, added with an organic solvent for crystallization, filtered and then dissolved in an aqueous solution, neutralized with hydrochloric acid, heated to dissolve and slowly cooled for crystallization, High purity ganciclovir is available.

[0026] Specifically include the following steps:

[0027] a, the ganciclovir crude product is adjusted pH to 13.0 with the sodium hydroxide aqueous solution of 6% with mass concentration, makes ganciclovir salify and is easily soluble in water, controls feed liquid volume to be about ganciclovir dry weight 2-4 times, keep stirring at 20°C for 60 minutes, add activated carbon with 10% weight of crude ganciclovir, stir for 1 hour, and filter; adding activated carbon can absorb some impurities and ensure the filtering effect to remove some insoluble impurities.

[0028] b. Heat the filtrate to 40°C, add dropwise the organic sol...

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PUM

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Abstract

The invention relates to a ganciclovir purification process, which specifically comprises the following steps: dissolving crude ganciclovir in alkaline solution, regulating pH, adding active carbon and conducting agitation and filtration; adding organic solvent in filtrate and filtering the obtained sediment; and dissolving filter cakes in deionized water, adding hydrochloric acid for neutralization, heating and dissolving the obtained sediment and then slowly decreasing temperature, and filtering and drying the produced crystals to obtain high-purity ganciclovir. Compared with the prior art, the invention has the advantages of simple operation, high yield, cost saving, reduced wastage in production, reduced environmental pollution and the like.

Description

technical field [0001] The invention relates to a refining process of antiviral drugs, in particular to a refining process of ganciclovir. Background technique [0002] Ganciclovir is an acyclic nucleoside antiviral drug, which is active against all herpes viruses, and its activity against E-B virus (EBV) and cytomegalovirus (CMV) is greater than that of acyclovir. Its mechanism of action is similar, and its selectivity to viruses is higher, but its toxicity to mammals is less; And anti-SARS virus etc. also have certain effect. Ganciclovir is a multi-step chemical reaction, and some process intermediate steps involve isomer resolution, so the yield is low-cost and high. The domestic process mainly uses 2,9-diacetylguanine as the starting material, and 1, 3-dichloromethoxyl-2-propoxymethanol acetate carries out condensation reaction, carries out esterolysis reaction with acetic anhydride again, hydrolyzes and refines to obtain Ganciclovir crude product, finally four crystal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18A61P31/12A61P31/22
Inventor 秦永忠王景立周曹芹
Owner SHANGHAI YIWEI INDAL
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