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Abacavir crystal and preparation method thereof

A crystal and X-ray technology, applied in the field of medicinal chemistry, can solve the problems that are not suitable for industrial production and large-scale preparation of preparations, and achieve the effects of easy operation and large-scale, high purity and stable form

Inactive Publication Date: 2016-02-10
SHANGHAI DESANO CHEM PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the abacavir obtained by these methods is solid, these solids will spontaneously transform into brown jelly or viscous after several hours, so they are not suitable for industrial production and large-scale preparation of preparations

Method used

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  • Abacavir crystal and preparation method thereof
  • Abacavir crystal and preparation method thereof
  • Abacavir crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 10g of abacavir to 30mL of N-methylpyrrolidone, heat up to dissolve; at 50-60°C, add 30mL of isopropyl ether dropwise; after dropping, keep stirring for 1-2 hours; slowly drop to At room temperature, the precipitated crystals were collected, washed with isopropyl ether, and then dried in vacuum at 40-50° C. to obtain 8.3 g of the abacavir crystals, with an HPLC purity of 99.35%.

[0034] figure 1 For the X-ray powder diffraction spectrum of the abacavir crystal obtained, by figure 1 It can be seen that the obtained abacavir crystals have main characteristic peaks at diffraction angles 2θ of 9.0°, 10.1°, 12.7°, 13.2°, 17.8°, 20.2°, 23.8°, and 25.5° under powder X-ray diffraction There are characteristic peaks at 9.0°, 10.1°, 12.7°, 13.2°, 14.5°, 17.8°, 18.5°, 20.2°, 23.8°, 25.5°, 27.1°, 29.0°, 35.9° at the diffraction angle 2θ.

[0035] figure 2 For the DSC spectrogram of the obtained abacavir crystals, by figure 2 It can be seen that the differential thermal a...

Embodiment 2

[0037] Add 10g of abacavir salicylate into 35mL of N-methylpyrrolidone, heat up to dissolve; at 50-60°C, add 50mL of isopropyl ether dropwise; after dropping, keep stirring for 1 to 2 hours Slowly lower to room temperature, collect the precipitated crystals, wash with isopropyl ether; then dry in vacuo at 40-50°C to obtain 7.1 g of the abacavir crystals, with an HPLC purity of 99.51%.

[0038] The abacavir crystals obtained in this embodiment also have figure 1 The powder X-ray diffraction pattern features shown and figure 2 Features of the DSC spectrum shown.

Embodiment 3

[0040] Add 10g of abacavir to 25mL of dimethyl sulfoxide (DMSO), heat up to dissolve; at 50-60°C, add 40mL of isopropyl ether dropwise; after dropping, keep stirring for 1-2 hours; Slowly lower to room temperature, collect the precipitated crystals, wash with isopropyl ether; then vacuum-dry at 40-50° C. to obtain 8.0 g of the abacavir crystals with an HPLC purity of 99.42%.

[0041] The abacavir crystals obtained in this embodiment also have figure 1 The powder X-ray diffraction pattern features shown and figure 2 Features of the DSC spectrum shown.

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Abstract

The invention discloses an abacavir crystal and a preparation method thereof. Under powder X-ray diffraction, the crystal has main characteristic peaks at the diffraction angle 2[theta] of 9.0 degrees, 10.1 degrees, 12.7 degrees, 13.2 degrees, 17.8 degrees, 20.2 degrees, 23.8 degrees and 25.5 degrees, wherein test error is + / - 0.2 degrees. The preparation method comprises the following steps: adding an abacavir raw material to an organic solvent, increasing the temperature until the solution is clear, dropwisely adding an anti-solvent at 50-60 DEG C, and then performing temperature-maintained stirring for 1-2 h, finally reducing the temperature to room temperature, collecting the separated-out crystal and drying the crystal. The abacavir crystal has stable form, is easy to separate, is high in purity and is stable in quality. The preparation method is simple in process, is easy to operate and achieve in large scale, and is beneficial to development and large-scale production of a follow-up preparation.

Description

technical field [0001] The invention relates to an abacavir crystal and a preparation method thereof, belonging to the technical field of medicinal chemistry. Background technique [0002] Abacavir is an antiretroviral drug launched by GlaxoSmithKline. It is a carbocyclic 2'-deoxyguanosine drug, which is an inactive precursor like other nucleoside reverse transcriptase inhibitors medicine. Its chemical structure is shown below: [0003] [0004] At present, reports on the forms of abacavir mainly include: anhydrous, amorphous and acetone, ethyl acetate solvate. Some literatures describe methods for isolating abacavir by grinding or chromatography, but the result is always a gum-like solid or solid foam, which is difficult to achieve industrial scale operation. [0005] WO9852949 describes the preparation of abacavir from acetone, during the preparation of abacavir free base an amorphous solid is produced which absorbs the solvent and is therefore not suitable for use w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/16
Inventor 李竟鹏赵楠王锰
Owner SHANGHAI DESANO CHEM PHARMA
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