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Sodium phenylacetate crystal form A, and preparation method and application thereof

A technology of sodium phenylacetate and phenylacetic acid, applied in the directions of carboxylate preparation, carboxylate preparation, amide preparation, etc., can solve problems such as limitation, low crystal purity of sodium phenylacetate, poor stability, etc. The method is simple and easy to operate, and the reaction conditions are mild.

Pending Publication Date: 2019-07-02
凯默斯医药科技上海有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low purity and poor stability of the sodium phenylacetate crystals prepared by the prior art, its application in the pharmaceutical and chemical industry is limited

Method used

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  • Sodium phenylacetate crystal form A, and preparation method and application thereof
  • Sodium phenylacetate crystal form A, and preparation method and application thereof
  • Sodium phenylacetate crystal form A, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation of embodiment 1 sodium phenylacetate crystal form A

[0027] Add 200 mL of hydrochloric acid (5 mol / L) and 136.2 g of phenylacetamide into the container, heat until the reaction is complete, and cool down to crystallize. Filter and dry. The dried solid was added into 280 mL of methylcyclohexane and heated until completely dissolved. Cool down to crystallize, filter, and dry under reduced pressure to obtain 102.1 g of phenylacetic acid with a yield of 75.0%.

[0028] Add 75mL sodium hydroxide solution (10mol / L) and 102.1g phenylacetic acid to the container, stir until the reaction is complete, concentrate to dryness to obtain crude sodium phenylacetate, then add a mixed solution of 510mL acetonitrile and 15mL water, heat and stir until Dissolved completely, cooling down to crystallize. After filtration and drying under reduced pressure, 117.5 g of white crystalline powder was obtained, namely sodium phenylacetate crystal form A. Yield 99.1%, chemical ...

Embodiment 2

[0031] The preparation of embodiment 2 sodium phenylacetate crystal form A

[0032] Add 450mL of hydrochloric acid (3mol / L) and 181.5g of phenylacetamide into the container, heat until the reaction is complete, and cool down to crystallize. Filter and dry. The dried solid was added into 370mL cyclohexane and heated until completely dissolved. Cool down to crystallize, filter, and dry under reduced pressure to obtain 136.0 g of phenylacetic acid with a yield of 74.9%.

[0033] Add 135mL sodium hydroxide solution (7.5mol / L) and 136.0g phenylacetic acid into the container, stir until the reaction is complete, concentrate to dryness to obtain crude sodium phenylacetate, then add 680mL acetone and 20mL water mixed solvent, heat and stir Until the dissolution is complete, cool down and crystallize. Filter and dry under reduced pressure to obtain 157.2 g of white crystalline powder, namely sodium phenylacetate crystal form A. Yield 99.5%, chemical purity 99.95%.

Embodiment 3

[0034] The preparation of embodiment 3 sodium phenylacetate crystal form A

[0035] Add 500mL of hydrobromic acid (4mol / L) and 272.3g of phenylacetamide into the container, heat until the reaction is complete, then cool down to crystallize. Filter and dry. The dried solid was added into 550mL cycloheptane and heated until completely dissolved. Cool down to crystallize, filter, and dry under reduced pressure to obtain 204.5 g of phenylacetic acid with a yield of 75.1%.

[0036] Add 300mL sodium bicarbonate solution (5mol / L) and 204.5g phenylacetic acid into the container, stir until the reaction is complete, and concentrate to dryness to obtain the crude sodium phenylacetate, then add a mixed solvent of 1000mL isopropanol and 30mL water, heat and stir Until the dissolution is complete, cool down and crystallize. Filter and dry under reduced pressure to obtain 235.3 g of white crystalline powder, namely sodium phenylacetate crystal form A. Yield 99.2%, chemical purity 99.97%...

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Abstract

The invention provides a sodium phenylacetate crystal form A. In X-ray powder diffraction of the crystal form, characteristic peaks exist at positions with 2-theta diffraction angles of 5.4+ / -0.2 degrees, 5.7+ / -0.2 degrees, 20.1+ / -0.2 degrees and 21.7+ / -0.2 degrees. The invention also provides a preparation method and application of the sodium phenylacetate crystal form A. Experimental results show that the sodium phenylacetate crystal form A is high in chemical purity and good in stability. Compared with a sodium phenylacetate crystal compound solution prepared in the prior art, the sodium phenylacetate solution prepared by the crystal form disclosed by the invention has better stability. In addition, the preparation method disclosed by the invention is simple and easy to operate, the reaction conditions are mild, the yield is greater than 99.0%, and the method is suitable for industrial production.

Description

technical field [0001] The present invention relates to sodium phenylacetate crystal form A and its preparation method and application. Background technique [0002] Sodium phenylacetate (C 8 h 7 o 2 Na), a white crystalline powder, is mainly used in the production of drugs such as penicillin in the pharmaceutical industry. Oral liquid and injection prepared by itself or in combination with sodium benzoate are used for treating hyperammonemia in patients with urea cycle disorder (UCD) and assisting in the treatment of related diseases. As an inhibitor of the ERK pathway, sodium phenylacetate has biological effects such as inducing the maturation, differentiation and apoptosis of various tumor cells, and its toxicity is very low; the research on its anticancer effect and its mechanism has been paid more and more attention, and has broad development prospects. [0003] At present, there are few literatures about the preparation of sodium phenylacetate, and most of them are...

Claims

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Application Information

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IPC IPC(8): C07C57/32C07C51/06C07C51/41A61K31/192A61P13/00
CPCC07C57/32C07C51/06C07C51/412C07B2200/13
Inventor 刘小蜂王奇刘善金宿磊傅霖陈刚
Owner 凯默斯医药科技上海有限公司
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