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Preparation method for atovaquone III type crystal

A technology for atovaquone and crystals, which is applied in the field of preparing atovaquone type III crystals, can solve the problem of low crystal purity of type III atovaquone, and achieve the effects of easy control of process conditions and simple operation.

Inactive Publication Date: 2015-12-16
SHANGHAI DESANO CHEM PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of type III atovaquone crystals prepared by this method is not high, and some type I crystals are mixed therein

Method used

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  • Preparation method for atovaquone III type crystal
  • Preparation method for atovaquone III type crystal
  • Preparation method for atovaquone III type crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] At room temperature, dissolve 10.0 g of atovaquone crude product in 150 mL of acetone, then cool down to 15°C, add 0.01 g of atovaquone type III seed crystals, keep stirring for crystallization (stir for about 2 hours), and filter with suction , collected crystals, washed with 50 mL of purified water, and dried in vacuum at 45° C. to obtain 9.73 g of atovaquone type III crystals, with a mass yield of 97.3% and an HPLC purity of 98.6%.

[0041] figure 1 For the X-ray powder diffraction spectrum of the obtained crystal of the present embodiment, by figure 1 It can be seen that the X-ray powder diffraction spectrum of the obtained crystal has characteristic peaks at 2θ=7.1, 9.3, 9.7, 12.8, 14.3, 14.9, 15.2, 18.7, 19.2 and 20.1°, which is the same as that reported in Chinese patent application CN1878741A The X-ray powder diffraction spectrum of atovaquone type III crystal is consistent within the error range.

[0042] figure 2 For the DSC spectrum of the obtained crysta...

Embodiment 2

[0044] At room temperature, dissolve 5.0 g of atovaquone crude product in 50 mL of dichloromethane, then cool down to 10° C., add 0.05 g of atovaquone type III seed crystals, keep stirring to crystallize (about 0.5 hours after stirring), The crystals were collected by suction filtration, washed with 50 mL of purified water, and dried in vacuum at 50° C. to obtain 4.93 g of atovaquone type III crystals with a mass yield of 97.6% and an HPLC purity of 98.9%.

[0045] After analysis, the obtained crystals were atovaquone type III crystals.

Embodiment 3

[0047] At room temperature, dissolve 25.0 g of atovaquone crude product in 100 mL of tetrahydrofuran, then cool down to 10 ° C, add 0.25 g of atovaquone type III seed crystals, keep stirring to crystallize (about 2 hours after stirring), and filter with suction , collected crystals, washed with 50 mL of purified water, and dried in vacuum at 50° C. to obtain 24.8 g of atovaquone type III crystals, with a mass yield of 98.0% and an HPLC purity of 99.1%.

[0048] After analysis, the obtained crystals were atovaquone type III crystals.

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Abstract

The invention discloses a preparation method for atovaquone III type crystal. The method comprises the following steps: dissolving an atovaquone crude product in an organic solvent at room temperature; cooling to crystallize, collecting crystal, and drying. The preparation method for high purity atovaquone III type crystal has low cost and high yield, and has great industrial value for preparing atovaquone III type crystal in large-scale manner.

Description

technical field [0001] The invention relates to a method for preparing atovaquone type III crystals, belonging to the technical field of medicinal chemistry. Background technique [0002] Malaria is one of the outstanding problems of public health in the world today, and it is the most widespread and harmful parasitic disease in the world. At present, there are many varieties of antimalarial drugs such as artemisinin, lumefantrine, and atovaquone. [0003] The chemical name of atovaquone is (3S)-2-hydroxy-3-[4-(4-chlorophenyl)cyclohexyl]-1,4-naphthalenedione [CAS: 95233-18-4], which The chemical structural formula is as follows: [0004] [0005] Atovaquone had been put on the market as early as the 1970s, but it gradually disappeared after the advent of other antimalarial drugs with good efficacy. Atovaquone received renewed attention after the combination of varaquinone and proguanil hydrochloride, maralone, was used for the treatment and prophylaxis of acute, uncomp...

Claims

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Application Information

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IPC IPC(8): C07C50/32C07C46/10
Inventor 李竟鹏赵楠张良
Owner SHANGHAI DESANO CHEM PHARMA
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