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Crystallization method of bepiridic acid intermediate

An intermediate, volume ratio technology, applied in the field of medicine, can solve the problems of low product purity and yield, remaining raw materials, lack of quality control of key intermediates, etc., and achieve the effect of reducing production costs

Pending Publication Date: 2022-05-06
GAN&LEE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the above synthetic route, the crude product of BPD-4 is crystallized and purified using the n-hexane / methyl tert-butyl ether (MTBE) system, and the purity and yield of the obtained product are low; and the lack of necessary quality control for key intermediates makes the subsequent reduction The reaction consumes a large amount of sodium borohydride, and the amount of sodium borohydride added is more than ten times that of the substrate, and after a long time of reaction, there are still raw materials remaining, so it is difficult to complete the reaction

Method used

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  • Crystallization method of bepiridic acid intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 10.5L of isopropyl acetate to 3.5kg of crude BPD-4, heat to 70°C and stir to dissolve, add 52.5L of n-heptane, stir and crystallize at 25°C, filter, and drain. The obtained wet product continued to repeat the crystallization twice according to the above-mentioned refining conditions, filtered, and sucked dry. After drying, 3.09 kg of off-white solid BPD-4 was obtained, with a yield of 92.0% and a purity of 97.11%.

Embodiment 2

[0025] Add 5.0L of ethyl acetate to 1.0kg of crude BPD-4, heat to 50°C and stir to dissolve, add 10.0L of n-hexane, stir and crystallize at 20°C, filter and drain. After drying, 0.9 kg of off-white solid BPD-4 was obtained, with a yield of 90.0% and a purity of 91.27%.

Embodiment 3

[0027] Add 2.0L of n-butyl acetate to 1.0kg of crude BPD-4, heat to 80°C and stir to dissolve, add 20.0L of cyclohexane, stir and crystallize at 30°C, filter, and drain. After drying, 0.85 kg of off-white solid BPD-4 was obtained, with a yield of 85.0% and a purity of 95.49%.

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Abstract

The invention discloses a crystallization method of a BPD-4 intermediate, i.e., 8-oxo-2, 2, 14, 14-tetramethyl pentadecanedioic acid (BPD-4), which comprises the following steps: adding a BPD-4 crude product into an ester solvent under a heating condition, dissolving, adding an alkane solvent, cooling, crystallizing, filtering and drying to obtain purified BPD-4, and the obtained product is high in purity, low in cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a crystallization method of bempedelic acid intermediate 8-oxo-2,2,14,14-tetramethylpentadecanedioic acid (BPD-4). Background technique [0002] Bempedoic Acid is an adenosine triphosphate-citrate lyase (ACL) inhibitor developed by Esperion Therapeutics of the United States. It was approved for marketing by the FDA on February 21, 2020, under the trade name Nexletol. Bempedic acid can reduce the biosynthesis of cholesterol by up-regulating low-density lipoprotein (LDL) receptors, and lower the level of high-density lipoprotein cholesterol (LDL-C), which can be used to treat dyslipidemia and reduce the risk of other cardiovascular diseases. Compared with the currently widely used statins in clinical practice, the advantage of bempedelic acid is that it is well tolerated and can be used in combination with statins for the treatment of LDL-C that cannot be controlled by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/347C07C51/43
CPCC07C51/43C07C59/347
Inventor 张一宁陈知庆韩福庆廖明明
Owner GAN&LEE PHARMA