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Recovery method of valsartan mother liquor

A recovery method and technology for valsartan, applied in the field of recovery of valsartan mother liquor, can solve the problems of large yield deviation, low repeatability, insignificant isomer separation effect, etc., so as to reduce the proportion and reduce energy consumption. and solvent loss, good quality of recovered product

Active Publication Date: 2015-05-13
SOLIPHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, repeated experiments by the inventor have confirmed that the method has relatively low repeatability, a large yield deviation, and the separation effect of isomers is not obvious.

Method used

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  • Recovery method of valsartan mother liquor
  • Recovery method of valsartan mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Choose the mother liquor after the valsartan recrystallization of production, concentrate to dryness, obtain the valsartan recovery crude product containing 10.0% D-type isomer (HPLC detection peak area method), its L-valsartan content is 52.2%. Add 23.0g of recovered crude product containing valsartan and 46.0g of 4-methyl-2-pentanone into a 250mL three-necked flask, heat up to 50°C and stir to dissolve, cool down to 15°C, keep warm for 2 hours, then cool to 0°C, keep warm After 10 hours, filter and dry to obtain 6.97 g of valsartan with a purity of 99.8%, a ratio of D-isomer of 0.21%, and a yield of 58%.

Embodiment 2

[0039] Choose the mother liquor after the valsartan recrystallization of production, concentrate to dryness, obtain the valsartan recovery crude product containing 20.0% D-type isomer (HPLC detection peak area method), its L-valsartan content is 46.5%. In the 500mL there-necked flask, add 23.0g containing valsartan and reclaim the crude product and the mixed solvent of 230.0g 4-methyl-2-pentanone and ethyl acetate (the mass ratio of 4-methyl-2-pentanone and ethyl acetate is 1:10), heat up to 50°C and stir to dissolve, cool down to 20°C, add 50 mg of seed crystals, keep warm for 8 hours, then cool to -5°C, keep warm for 5 hours, shake off, and dry to obtain 4.50g of valsartan, The purity is 99.8%, the proportion of D-isomer is 0.3%, and the yield is 42%.

Embodiment 3

[0041]1, choose the mother liquor after the valsartan recrystallization of production, concentrate to dryness, obtain the valsartan recovery crude product containing 18.0% D type isomer (HPLC detection peak area method), its L-valsartan content is 44.4 %. Add 23.0g of recovered crude product containing valsartan and 46.0g of 4-methyl-2-pentanone into a 250mL three-necked flask, heat up to 50°C and stir to dissolve, cool down to 20°C, keep warm for 2 hours, then cool to -5°C, Keep warm for 2 hours, shake off and filter to obtain 17.8g of wet product. After a small amount of wet product was dried and tested, the purity was 98.8%, and the ratio of D-type isomer was 0.7%.

[0042] 2. Disperse 17.8 g of the wet product obtained in 1 in 17.8 g of ethyl acetate, soak for 40 minutes at 0° C., shake off to obtain 10.6 g of the wet product, and vacuum-dry to obtain 4.70 g of the refined product of valsartan. . A small amount of wet product was taken and tested after drying. The purit...

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Abstract

The invention relates to a recovery method of a valsartan mother liquor and belongs to the technical field of medical chemistry. The recovery method comprises the steps of dissolving the valsartan coarse product into a solvent containing 4-methyl-2-pentanone, heating till completely dissolving, cooling in stages for crystallization, and filtering to obtain valsartan solid. The purity of the valsartan mother liquor is greater than 99.8%, and the total recovery rate of the valsartan mother liquor is greater than or equal to 42%. For the valsartan coarse product having the isomer D-valsartan proportion within the range of 10% to 35%, the recovery method is capable of effectively reducing the isomer proportion, increasing the utilization rate of the valsartan and reducing the cost.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for recovering valsartan mother liquor. Background technique [0002] Valsartan (Valsartan), chemical name: N-(1-pentanoyl)-N-[4-[2-(1H-tetrazol-5-yl)phenyl]benzyl]-L-valline Acid is a non-peptide AII receptor antagonist, as a high blood pressure drug, it has a long acting time and good tolerance. [0003] [0004] In order to reduce costs, enterprises generally reclaim part of L-valsartan from the refined mother liquor, but when the ratio of D-valsartan in the valsartan mother liquor (HPLC detection peak area method) exceeds 10%, there is no suitable The method can recover qualified valsartan. The current refining process of valsartan has stricter requirements on the content of D-valsartan in the raw material. In the method for refining valsartan disclosed in the patent CN103435567, the isomer content of the raw materials used is 1.0-10.0%. Patent C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 陈冬冬盛晓霞
Owner SOLIPHARMA
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