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Preparation method of pitavastatin calcium by recrystallization

A technology of pitavastatin calcium and recrystallization, applied in the field of medicine

Inactive Publication Date: 2012-09-05
FOSHAN DAYI TECH LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims at the problems existing in the preparation of pitavastatin calcium at present, and provides a method for preparing pitavastatin calcium recrystallization to solve the above problems

Method used

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  • Preparation method of pitavastatin calcium by recrystallization
  • Preparation method of pitavastatin calcium by recrystallization

Examples

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Embodiment 1

[0026]

[0027] formula two

[0028] As reaction formula 2, add 134.93g (0.3mol) of compound I in a 2000ml flask, 1500ml absolute ethanol, stir to dissolve, cool to 0-4°C, drop 320ml of 1mol / L sodium hydroxide solution, and continue stirring for 3 hours to complete the hydrolysis reaction. Evaporate the solvent under reduced pressure, add 2000ml of water, stir to dissolve, and prepare pitavastatin sodium salt solution.

[0029] Add 16.65 g (0.15 mol) of calcium chloride 100 ml aqueous solution dropwise to the prepared pitavastatin sodium salt solution, continue stirring for 12 hours, filter, and dry to obtain pitavastatin calcium 126.8 g, yield 96%, HPLC purity 94% .

Embodiment 2

[0031] Add 134.93g (0.3mol) of compound I in a 2000ml flask, 1500ml absolute ethanol, stir to dissolve, cool to 0-4°C, drop 320ml of 1mol / L sodium hydroxide solution, and continue stirring for 3 hours to complete the hydrolysis reaction . Evaporate the solvent under reduced pressure, add 2000ml of water, stir to dissolve, and prepare pitavastatin sodium salt solution.

[0032] Add 400ml of tetrahydrofuran to the prepared pitavastatin sodium salt solution, drop in 100ml of aqueous solution of 16.65g (0.15mol) of calcium chloride, continue stirring at -0.08MPa for 12 hours to remove tetrahydrofuran by volatilization, filter, and dry to obtain pitavastatin Calcium 124.22g, yield 94%, HPLC purity 98%.

Embodiment 3

[0034] Add 100ml of tetrahydrofuran to 20g of pitavastatin calcium, stir to dissolve, add 400ml of water, continue to stir at -0.08MPa for 12 hours to volatilize and remove tetrahydrofuran, filter and dry to obtain 18.2g of pitavastatin calcium, yield 91%, HPLC purity 98 %.

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Abstract

The invention relates to the technical field of medicine, particularly a preparation method of pitavastatin calcium by recrystallization. The method is implemented in a way that: pitavastatin calcium is dissolved in a tetrahydrofuran / water mixed solvent, wherein the solubility is high; and after gradually removing the tetrahydrofuran by volatilization, since the solubility of the pitavastatin calcium in water is very low, the pitavastatin calcium gradually crystallizes and precipitates, thereby obtaining the pitavastatin calcium solid with favorable crystal form and also refining and purifying the pitavastatin calcium.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for preparing pitavastatin calcium recrystallization. Background technique [0002] Pitavastatin calcium, the chemical name is bis[(3R,5S,6E)-7-(2-cyclopropyl-4-(4-fluorophenyl)-3-quinolyl)-3,5-dihydroxy -6-heptenoic acid] monocalcium, the structural formula is as formula one: [0003] [0004] formula one [0005] Pitavastatin calcium, as a hydroxymethylglutaryl coenzyme A (HMG-CoA) reductase inhibitor, is clinically used to treat hyperlipidemia. It was registered in Japan in November 1999 and approved for marketing in July 2003. It not only has the advantages of other statin drugs, but also has shorter onset time, lower dosage, less side effects, better tolerance, and has a good market prospect. [0006] It is usually reported that the synthesis of pitavastatin calcium is all about adding calcium chloride aqueous solution to the sodium salt solution of pitavasta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/14
Inventor 唐良伟雍智全闻亚磊雷安胜伍伟成曾树泽
Owner FOSHAN DAYI TECH LTD
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