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Preparation method of high-purity tenofovir

A tenofovir, high-purity technology, applied in the field of chemical drug synthesis, can solve the problem that the product purity is only 99.3%

Active Publication Date: 2018-08-03
科兴生物制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Patent CN107573381A discloses a one-pot method for preparing tenofovir, the method is simple, but the product purity is only 99.3%

Method used

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  • Preparation method of high-purity tenofovir

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preparation example Construction

[0033] The present invention provides a kind of preparation method of high-purity tenofovir, at least comprises the following steps:

[0034] (1) Add R-1,2-propanediol, diethyl carbonate and sodium ethylate to the reactor, heat, keep warm and react, and the reaction is terminated. Unreacted diethyl carbonate is steamed out by distillation under reduced pressure, cooled to room temperature, The insoluble matter was filtered off, and concentrated to dryness under reduced pressure to obtain R-propylene carbonate;

[0035] (2) add toluene, catalyzer in reactor, carry out rectifying column rectification 6-8h, after rectifying completes, decompress and concentrate dry, obtain the catalyst with high purity;

[0036] (3) Mix adenine and R-propylene carbonate in the first solvent under the protection of nitrogen, under alkali catalysis, heat, heat preservation reaction, reaction termination, obtain 9-(2-hydroxypropyl) adenine crude product, filter , concentrating under reduced pressur...

Embodiment 1

[0088] The preparation method of high-purity tenofovir at least comprises the following steps:

[0089] (1) Add R-1,2-propanediol, diethyl carbonate and sodium ethoxide to the reactor, heat to 105-108°C, keep warm for 8 hours, the reaction is terminated, and the unreacted diethyl carbonate is distilled under reduced pressure. out, cooled to room temperature, filtered off insoluble matter, concentrated to dryness under reduced pressure to obtain R-propylene carbonate; the molar ratio of the R-1,2-propanediol to the diethyl carbonate and the sodium ethoxide was 1:1.15 : 0.82;

[0090] (2) add toluene, catalyzer in reactor, carry out rectifying column rectification 6-8h, after rectifying completes, decompression concentrates dry, obtains the catalyst that purity is high; The weight ratio of described toluene and described catalyzer is 11 : 1; the catalyst is potassium tert-butoxide;

[0091] (3) Mix adenine and R-propylene carbonate in the first solvent under the protection of ni...

Embodiment 2

[0096] The preparation method of high-purity tenofovir at least comprises the following steps:

[0097] (1) Add R-1,2-propanediol, diethyl carbonate and sodium ethoxide to the reactor, heat to 105-108°C, keep warm for 8 hours, the reaction is terminated, and the unreacted diethyl carbonate is distilled under reduced pressure. out, cooled to room temperature, filtered off insoluble matter, concentrated to dryness under reduced pressure to obtain R-propylene carbonate; the molar ratio of the R-1,2-propanediol to the diethyl carbonate and the sodium ethoxide was 1:1.15 : 0.82;

[0098] (2) add toluene, catalyzer in reactor, carry out rectifying column rectification 6-8h, after rectifying completes, decompression concentrates dry, obtains the catalyst that purity is high; The weight ratio of described toluene and described catalyzer is 11 : 1; the catalyst is potassium tert-butoxide;

[0099] (3) Mix adenine and R-propylene carbonate in the first solvent under the protection of ...

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Abstract

The invention provides a preparation method of high-purity tenofovir. The method at least comprises the following steps: (1) preparing R-propylene carbonate; (2) purifying a catalyst; (3) carrying outcondensation reaction on adenine with R-propylene carbonate; (4) carrying out etherification reaction on 9-(2-hydroxypropyl) adenine with diethyl p-toluenesulfonyloxymethylphosphonate; (5) carrying out hydrolysis reaction on tenofovir diester; and (6) refining crude tenofovir.

Description

technical field [0001] The invention relates to the technical field of chemical drug synthesis, in particular, the invention relates to a preparation method of high-purity tenofovir. Background technique [0002] The chemical name of tenofovir (tenofovir) is (R)-9-(2-phosphomethoxypropyl)-adenine, which is the key intermediate of the antiviral drug tenofovir disoproxil fumarate. Tenofovir disoproxil fumarate, the chemical name is 5-[[(1R)-2-(6-amino-9H-purin-9-yl)-1-methylethoxy]methyl]-2, 4,6,8-tetraoxo-5-phosphazelate diisopropyl-5-oxide fumarate is a nucleotide reverse transcriptase inhibitor developed by Gilead Sciences in the United States. The prodrug of fovir (PMPA), first listed in the United States in 2001, is mainly used clinically for the treatment of human immunodeficiency virus (HIV) infection, and can be used in conjunction with other antiretroviral drugs. [0003] At present, the preparation of relevant tenofovir mainly contains the following several methods...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6561
CPCC07F9/65616
Inventor 崔宁郝志海张允王君郭超任世平王翠翠仇渡先
Owner 科兴生物制药股份有限公司
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