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The crude product purification method of 1,2,4-triazole-3-carboxylic acid methyl ester

A technology of methyl carboxylate and purification method, applied in the field of crude product purification of 1,2,4-triazole-3-carboxylate methyl ester, can solve the problem of uneven particle size, affecting product application, poor transparency, etc. problem, to achieve the effect of white crystal appearance, improved drug yield, and uniform crystal appearance

Active Publication Date: 2015-09-02
SHANDONG YANGCHENG BIOLOGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The finished product still contains some impurities, the appearance of the crystal is light yellow, the transparency is poor, and the particle size is uneven, so the purity of the crystal has been 92-94%, which affects the application of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Re-dissolution of the wet crude product: In the current production process of 1,2,4-triazole-3-carboxylate methyl ester, after the wet crude product crystallized by nitrogen release and suction filtration, methanol with 15 times the volume of the wet crude product was used Solvent, re-dissolve the obtained wet crude crystals at 70°C;

[0021] (2) Activated carbon decolorization: Add activated carbon accounting for 10% of the volume of methanol solvent to the solvent, and keep it for 15 minutes for decolorization;

[0022] (3) Temperature-controlled recrystallization: Control the temperature of the solvent to drop slowly to 50°C, add seed crystals accounting for 1% of the weight of the wet crude product, and then control the temperature to slowly drop to 35°C to re-form white crystals with uniform particles;

[0023] (4) Dry the crystals to obtain the finished product, and the purity of the product is 99.6%.

Embodiment 2

[0025] (1) Redissolution of the wet crude product: In the current production process of methyl 1,2,4-triazole-3-carboxylate, after the crystallization of the wet crude product obtained by nitrogen release and suction filtration, methanol with 13 times the volume of the wet crude product is used Solvent, re-dissolve the obtained wet crude crystals at 70°C;

[0026] (2) Activated carbon decolorization: Add activated carbon accounting for 7% of the volume of methanol solvent to the solvent, and keep it for 20 minutes for decolorization;

[0027] (3) Temperature-controlled recrystallization: Control the temperature of the solvent to drop slowly to 50°C, add seed crystals accounting for 1% of the weight of the wet crude product, and then control the temperature to slowly drop to 35°C to re-form white crystals with uniform particles;

[0028] (4) Dry the crystals to obtain the finished product, and the purity of the product is 99.8%.

Embodiment 3

[0030] (1) Redissolution of the wet crude product: In the current production process of methyl 1,2,4-triazole-3-carboxylate, after the crystallization of the wet crude product obtained by nitrogen release and suction filtration, methanol with 10 times the volume of the wet crude product is used Solvent, re-dissolve the obtained wet crude crystals at 70°C;

[0031] (2) Activated carbon decolorization: Add activated carbon accounting for 5% of the volume of methanol solvent to the solvent, and keep it for 24 minutes for decolorization;

[0032] (3) Temperature-controlled recrystallization: Control the temperature of the solvent to drop slowly to 50°C, add a seed crystal accounting for 0.5% of the weight of the wet crude product, and then control the temperature to slowly drop to 35°C to re-form white crystals with uniform particles;

[0033] (4) Dry the crystals to obtain the finished product, and the purity of the product is 99.7%.

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PUM

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Abstract

The invention belongs to the field of medical intermediate preparation, and especially relates to a method used for purifying methyl 1, 2, 4-triazole-3-carboxylate coarse product. The wet methyl 1, 2, 4-triazole-3-carboxylate coarse product prepared by acylation, cyclization, esterification, diazotization and nitrogen-releasing suction filtration is used as a raw material. The method used for purifying the methyl 1, 2, 4-triazole-3-carboxylate coarse product comprises following steps: the wet coarse product is re-dissolved in methanol solvent; active carbon is added for decoloration; temperature reduction is controlled for recrystallization; and wet crystals obtained after recrystallization is dried so as to obtain finished products. The steps of the method are simple; the coarse product is re-dissolved, active carbon is used for adsorption, and temperature is controlled for recrystallization, so that the finished products with high purity and uniform crystals are obtained, and the finished products are of significant benefits on improvement of the quality of later produced medicine products, and are suitable for wide popularization and application.

Description

(1) Technical field [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to a crude product purification method of methyl 1,2,4-triazole-3-carboxylate. (2) Background technology [0002] Methyl 1,2,4-triazole-3-carboxylate, the chemical name is 1H-1,2,4-methyl triazole-3-carboxylate, alias: methyl triazolecarboxylate, nucleus Glycoside, the molecular formula is C 4 h 5 N 3 o 2 , the structural formula is: , the molecular weight is 127.10. [0003] Methyl 1,2,4-triazole-3-carboxylate is an important intermediate of the antiviral drug ribavirin, and its different production processes lead to differences in yields, which directly affect the production of ribavirin; , the technological route of methyl triazole carboxylate produced in my country is: acylation → cyclization → esterification → diazo → nitrogen release suction filtration → drying and packaging. [0004] The original crystallization of the finished product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/10
Inventor 王东阳高杰闫如东徐强金光
Owner SHANDONG YANGCHENG BIOLOGY TECH CO LTD
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