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A kind of preparation method of ganciclovir

A technology of ganciclovir and triacetyl, applied in the field of preparation of ganciclovir, can solve the problem that the quality of ganciclovir is low, the main purity can only reach 99.0%, the yield and quality of triacetyl ganciclovir products Low problems, to achieve the effect of no toxicity and danger, low production cost, and simplified operation

Active Publication Date: 2021-03-26
武汉华龙生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages: calculated by diacetylguanine, the total yield is only 6.8% to 26.8%; the quality of finished product ganciclovir is low, EP impurity F (guanine) can only be controlled at about 0.5%, and the main purity can only reach About 99.0%
Therefore, in summary, present stage triacetylganciclovir production technology mainly also exists the problem that triacetylganciclovir product yield and quality are low

Method used

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  • A kind of preparation method of ganciclovir

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Embodiment 1

[0025] Embodiment 1 of the present invention provides a kind of preparation method of ganciclovir, comprises the steps:

[0026] Step 1: Synthesis of Triacetylganciclovir

[0027] Put 30.0g of diacetylguanine, 120ml of dioxane, 61.0g of glyceryl acetal and 2.3ml of trifluoroacetic acid into a 500ml three-necked bottle, heat to 80°C in an oil bath under stirring, react for 50h, and track the reaction by TLC [developer : Chloroform: methyl alcohol=85: 15], cool to 20 ℃ after reaction finishes, filter, filter cake is washed with 20ml dioxane, add in methanol (50ml), be heated to 60 ℃, stir to make it dissolve, filter, The filtrate was cooled to 0°C and crystallized for 30 minutes, filtered, and the filter cake was dried at 60-80°C for 5 hours to obtain 14.0 g of light yellow crude product I of triacetylganciclovir. The filtrate was concentrated to dryness under reduced pressure, and the residue was added to 100ml of a mixed solvent of methanol: ethyl acetate = 1:4, heated to 60°...

Embodiment 2

[0039] Embodiment 4 of the present invention provides a kind of preparation method of ganciclovir, except that step 3 is changed to "the volume-to-weight ratio of the ethanol aqueous solution and the crude product of ganciclovir is 75:1; the unit of the volume-to-mass ratio Be ml / g; The weight of described gac is except the 2.5% of Ganciclovir crude product weight ", all the other are all the same as embodiment 1.

Embodiment 3

[0041] Embodiment 4 of the present invention provides a kind of preparation method of ganciclovir, except that step 3 is changed to "the volume-to-weight ratio of the ethanol aqueous solution and the crude product of ganciclovir is 85:1; the unit of the volume-to-mass ratio Be ml / g; The weight of described gac is except the 5% of Ganciclovir crude product weight ", all the other are all with embodiment 1.

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Abstract

The invention provides a ganciclovir preparation method, which comprises: 1, carrying out a condensation reaction process by adopting glycerol acetal ester and diacetyl guanine as raw materials and dioxane as a solvent under the effect of trifluoroacetic acid, and carrying out post-treatment to obtain triacetyl ganciclovir, 2, hydrolyzing the triacetyl ganciclovir obtained in the step 1 to obtaina ganciclovir crude product, and 3, refining the ganciclovir crude product obtained in the step 2 to obtain a ganciclovir finished product. According to the method, based on diacetyl guanine, the total yield reaches 35%-40%, the quality of the prepared bulk drug product is greatly improved, the contents of the impurity C and the impurity F (guanine) are controlled to 0.05% or below, the total impurity content is 0.06%-0.10%, and the product purity is greater than 99.9%.

Description

technical field [0001] The invention relates to the technical field of substance synthesis, in particular to a preparation method of ganciclovir. Background technique [0002] Ganciclovir is the second-generation nucleoside antiviral drug. It is mainly used for the treatment and prevention of cytomegalovirus infection in clinical practice. The indications are cytomegalovirus retinitis, AIDS, organ transplantation, Malignant tumors, etc., as well as patients with pneumonia, gastroenteritis, liver and central nervous system CMV infection, compared with traditional antiviral drugs, it has the advantages of better efficacy and less side effects. [0003] Regarding the preparation method of ganciclovir, Syntex, the original research company in the United States, uses 1,3-dibenzyloxy-2-propoxy acetate, and then condenses with diacetylguanine to separate isomers, and palladium carbon catalyzes hydrogen Liberation of benzyl to obtain ganciclovir. There are disadvantages: calculate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/18
CPCC07D473/18
Inventor 丁冠军刘薇黄楚华吴芬董辉
Owner 武汉华龙生物制药有限公司
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