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Preparation method of O-monoacetyl ganciclovir

A technology of ganciclovir and monoacetyl, which is applied in the field of preparation of O-monoacetyl ganciclovir, can solve the problems of difficult removal of ganciclovir, difficulty in removing ganciclovir, and troublesome handling, and achieves short process steps. , The effect of reducing production cost and less impurities

Active Publication Date: 2021-03-16
沃德药业(安徽)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The raw material ganciclovir of the above-mentioned first process is difficult to react completely, and it is difficult to remove the ganciclovir after adding water for reverse hydrolysis, and it is troublesome to deal with after recovery; the second process is longer and the cost is higher

Method used

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  • Preparation method of O-monoacetyl ganciclovir
  • Preparation method of O-monoacetyl ganciclovir

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] S1. Put 40kg of triacetylganciclovir and 120kg of pyridine into a 500L reaction kettle, add 4kg of water, stir and heat up to 70°C;

[0028] S2, sampling detection (HPLC) after 12 hours of incubation reaction, detection result is as follows figure 1 and Table 1, by figure 1 As can be seen from Table 1, the content of monoacetylganciclovir is obviously increasing, and the content of triacetylganciclovir is declining;

[0029] S3. After 36 hours of heat preservation reaction, sampling and testing were carried out, and the test results were as follows: figure 2 and Table 2, by figure 2 As can be seen from Table 2, the insulation reaction has reacted completely;

[0030] S4. Heating up to 100° C. and depressurizing, collecting evaporated water vapor and pyridine. At this time, the liquid main reactant and part of water are retained in the reactor, and then the pyridine is evaporated to dryness under reduced pressure for recycling;

[0031] S5, add 200kg ethyl acetate ...

Embodiment 2

[0039] S1. Put 40kg of triacetylganciclovir and 120kg of piperidine into a 500L reaction kettle, add 4kg of water, stir and heat up to 80°C;

[0040] S2, sampling and detection (HPLC) after 12 hours of heat preservation reaction, half of the reaction is completed;

[0041] S3. After 36 hours of heat preservation reaction, sampling and testing were performed, and the reaction was complete;

[0042] S4. Warming up to 90° C. and reducing pressure, collecting evaporated water vapor and piperidine. At this time, the liquid main reactant and part of water are retained in the reactor, and then the piperidine is evaporated to dryness under reduced pressure for recycling;

[0043] S5, add 200kg ethyl acetate to the reaction kettle, stir and reflux for 3 hours, cool down and crystallize;

[0044] S6, centrifugal treatment, after solid-liquid separation is realized, the solid is collected and dried to obtain 29.6 kg of O-monoacetylganciclovir finished product; the liquid is collected, d...

Embodiment 3

[0047] S1. Put 40kg of triacetylganciclovir and 120kg of N-methylmorpholine into a 500L reactor, add 4kg of water, stir and heat up to 75°C;

[0048] S2, sampling and detection (HPLC) after 12 hours of heat preservation reaction, the reaction has not been completed yet;

[0049] S3, take a sample after 40 hours of heat preservation reaction, and the reaction is complete;

[0050] S4. Heating up to 95°C and depressurizing, collecting the evaporated water vapor and N-methylmorpholine. At this time, the liquid main reactant and part of water are kept in the reaction kettle, and then the N-methylmorpholine is decompressed separately Evaporate to dryness and recycle;

[0051] S5, add 200kg ethyl acetate to the reaction kettle, stir and reflux for 3 hours, cool down and crystallize;

[0052] S6. Centrifuge and dry to obtain 29.5 kg of O-monoacetylganciclovir finished product, and distill to recover ethyl acetate.

[0053] It can be calculated that the yield of O-monoacetylgancicl...

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Abstract

The invention discloses a preparation method of O-monoacetyl ganciclovir, and belongs to the technical field of medicine preparation. According to the preparation method, triacetyl ganciclovir is usedas a raw material, an organic weak base is used as a solvent and used as an alkaline hydrolysis condition at the same time, direct hydrolysis can be performed under a small amount of water, time andtemperature are controlled, it can be seen through HPLC-based reaction process monitoring that the content of monoacetyl ganciclovir is obviously increased and the content of triacetyl ganciclovir isreduced, after the reaction is finished, evaporation is performed under reduced pressure to remove the solvent, ethyl acetate is added, stirring and crystallizing are carried out, and centrifugal drying is carried out to obtain a finished product; and solvent steam is collected and subjected to reduced-pressure evaporation drying, then the solvent can be recycled, and ethyl acetate can be recycledafter filtrate obtained through centrifugal separation is distilled. The raw materials are cheap and easily available, the reaction is easy to complete, and the post-treatment is relatively simple; and the method has the advantages of simple reaction process, short process steps, low production cost, high finished product conversion rate and no environmental pollution, is more suitable for industrial production than the traditional process, and better conforms to the concept of green chemistry.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, in particular to a preparation method of O-monoacetylganciclovir. Background technique [0002] Valganciclovir is a synthetic 2-deoxyguanosine analog, which is the prodrug of the antiviral drug ganciclovir (ganciclovir), which can greatly reduce the toxicity of ganciclovir. Its pharmacodynamic characteristics are the same as ganciclovir. After oral administration, valganciclovir is rapidly hydrolyzed into ganciclovir under the action of intestinal mucosal cell esterase and liver esterase, and ganciclovir is phosphorylated by intraviral and intracellular enzymes to generate ganciclovir triphosphate , the latter competes with deoxyguanosine triphosphate (dGTP) as a substrate for viral DNA polymerase, thus inhibiting the synthesis of viral DNA, resulting in anti-CMV activity. As one of the main raw materials of valganciclovir, O-monoacetylganciclovir is widely used, and there are two ...

Claims

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Application Information

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IPC IPC(8): C07D473/18
CPCC07D473/18Y02P20/582
Inventor 何亚奇钟俊生
Owner 沃德药业(安徽)股份有限公司
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