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A kind of abacavir intermediate and purification method thereof

A purification method and intermediate technology, applied in the field of abacavir intermediates and its purification, can solve the problems of unfavorable industrial production and complicated methods, and achieve the effects of low cost, simple operation and easy control

Active Publication Date: 2020-06-26
SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The prior art usually adopts the method of column chromatography to obtain high-purity abacavir intermediate IV, however, the inventors of the present application found in the long-term research and development process that this method is relatively complicated and is not conducive to industrial production

Method used

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  • A kind of abacavir intermediate and purification method thereof
  • A kind of abacavir intermediate and purification method thereof
  • A kind of abacavir intermediate and purification method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Add 50g of the crude abacavir intermediate to 300mL of methanol, stir at room temperature for 30 minutes, and add 100mL of purified water during the stirring process, then heat at 50-60°C and stir until the crude abacavir intermediate is dissolved, then Add 0.5g of activated carbon, keep it warm under stirring for 1 hour, filter, and cool the filtrate to 8-12°C, crystallize for 3-6 hours, then filter and dry to obtain 34.8g off-white abacavir intermediate . Wherein, the mass yield of the obtained abacavir intermediate is 69.6%; the HPLC purity is 99.65%, and the absorbance (λ＝420nm) =0.01, absorbance (λ＝450nm) = 0.02.

Embodiment 2

[0062] Add 50g of the crude abacavir intermediate to 300mL of ethanol, stir at room temperature for 30 minutes, add 100mL of purified water, then heat at 50-60°C and stir until the crude abacavir intermediate is dissolved, then add 0.5g of activated carbon, It was kept under stirring for 1 hour, filtered, and the filtrate was cooled to 8-12° C., crystallized for 3-6 hours, then filtered and dried to obtain 36.1 g of off-white abacavir intermediate. Wherein, the mass yield of the abacavir intermediate obtained is 72.2%; HPLC purity 99.55%, absorbance (λ＝420nm) =0.02, absorbance (λ＝450nm) = 0.02.

Embodiment 3

[0064] Add 50g of the crude abacavir intermediate to 300mL of acetone, stir at room temperature for 30 minutes, add 100mL of purified water, then heat at 50-60°C and stir until the crude abacavir intermediate is dissolved, then add 0.5g of activated carbon, It was kept under stirring for 1 hour, filtered, and the filtrate was cooled to 8-12° C., crystallized for 3-6 hours, then filtered and dried to obtain 35.5 g of off-white abacavir intermediate. Wherein, the mass yield of the obtained abacavir intermediate is 71.0%; HPLC purity 99.70%, absorbance (λ＝420nm) =0.02, absorbance (λ＝450nm) = 0.02.

[0065] Specifically, the electron microscope pictures of the pure abacavir intermediate obtained in this embodiment are as follows: Figure 5 Shown; The absorbance value test result of abacavir intermediate pure product is as follows Figure 6 Shown, where the abscissa is the wavelength in nm; the ordinate is the absorbance.

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Abstract

The invention discloses an abacavir intermediate and a method for purifying the same. The method includes heating mixtures with abacavir intermediate crude products, purified water and water-soluble organic solvents until the abacavir intermediate crude products are completely dissolved so as to obtain mixed liquid; carrying out cooling and crystallization treatment on the mixed liquid; carrying out filtering and drying treatment after crystallization treatment is carried out so as to obtain abacavir intermediate pure products. A structural formula of the abacavir intermediate is shown as a formula IV. The abacavir intermediate and the method have the advantage that the method is easy and convenient to implement and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of compound purification, in particular to an abacavir intermediate and a purification method thereof. Background technique [0002] Abacavir is an effective selective inhibitor of HIV-1 and HIV-2, which can be used for the treatment of human immunodeficiency virus (HIV) infection. At present, there are many preparation methods related to abacavir, and in these methods, the most critical abacavir intermediate involved is shown in the following formula IV: [0003] [0004] In the prior art, column chromatography is usually used to obtain high-purity abacavir intermediate IV. However, the inventors of the present application have found in the long-term research and development process that this method is relatively complicated and is not conducive to industrial production. Contents of the invention [0005] The main technical problem to be solved by the present invention is to provide an abacavir interm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/40
Inventor 卜永海唐祁匀徐锦贾雪丁屏李海峰李春刚陈婷婷
Owner SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD
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