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Preparation and crystallization method of (2S)-2-animo-3-methyl-3-sulfinobutanoic acid

A technology of sulfinylbutyric acid and methyl group, which is applied in the field of preparation and crystallization of 2-amino-3-methyl-3-sulfinylbutyric acid, can solve the problem that the product is not easy to separate, unsuitable for long-term storage, complicated to operate, etc. problems, to achieve the effect of high product yield, easy storage, and high product purity

Inactive Publication Date: 2013-03-27
JIANGXI FUSHINE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by the present invention is to overcome problems such as many by-products, low purity, cumbersome operation, difficult separation of products, instability, and unfavorable long-term preservation in existing synthesis and separation technologies, and to provide a new (2S)2 -Amino-3-methyl-3-sulfinyl butanoic acid preparation and crystallization method

Method used

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  • Preparation and crystallization method of (2S)-2-animo-3-methyl-3-sulfinobutanoic acid
  • Preparation and crystallization method of (2S)-2-animo-3-methyl-3-sulfinobutanoic acid
  • Preparation and crystallization method of (2S)-2-animo-3-methyl-3-sulfinobutanoic acid

Examples

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Effect test

Embodiment 1

[0036] Put 150ml of ethanol and 15g of sodium hydroxide into a 500ml flask, cool to below 20°C, add 23.3g of sulbactam acid, dissolve heat, control the temperature at 20-25°C, react for 2h, the reaction is over, cool to 10°C, stir 1h, filter, rinse with appropriate amount of ethanol, dry under reduced pressure at 20-30℃ for 3h to obtain (2S)2-amino-3-methyl-3-sulfinylbutyric acid (also known as sulbactam penicillamine) 15.5g, 98.6% purity (see figure 1 , Where peak A is (2S)2-amino-3-methyl-3-sulfinylbutyric acid), the yield is 85.5%.

Embodiment 2

[0038] Put 300ml of ethanol and 20g of potassium hydroxide into a 500ml flask, lower the temperature to below 20°C, add 23.3g of sulbactam acid, dissolve exothermic, control the temperature at 20-30°C, react for 4h, the reaction is over, cool to 10°C, stir 1h, filter, rinse with appropriate amount of ethanol, dry under reduced pressure at 20-30℃ for 3h to obtain (2S)2-amino-3-methyl-3-sulfinylbutyric acid (also known as sulbactam penicillamine) 16.0g, purity 96%, yield 88.4%.

Embodiment 3

[0040] Put 150ml of ethanol and 16g of sodium hydroxide into a 500ml flask, lower the temperature to below 20°C, add 25.5g of sulbactam sodium, dissolve heat, control the temperature at 20-25°C, react for 5h, the reaction is over, cool to 5°C, stir 1h, filter, rinse with appropriate amount of ethanol, dry under reduced pressure at 20-30℃ for 3h to obtain (2S)2-amino-3-methyl-3-sulfinylbutyric acid (also known as sulbactam penicillamine) 16.0g, purity 96%, yield 88.4%.

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Abstract

The invention provides a preparation and crystallization method of (2S)-2-animo-3-methyl-3-sulfinobutanoic acid. The preparation and crystallization method comprises the following steps of: with salbactam acid or salbactam salt as an initial raw material, adding alkali to an organic solvent, directly filtering and separating after the reaction is completed, and then drying to obtain the (2S)-2-animo-3-methyl-3-sulfinobutanoic acid. The (2S)-2-animo-3-methyl-3-sulfinobutanoic acid (salbactam penicillamine) prepared by using the preparation and crystallization method has the purity of being more than 95 percent, meets the requirements as an impurity standard substance and plays an active role in search and detection of salbactam-related impurities.

Description

Technical field [0001] The invention relates to a preparation and crystallization method of (2S) 2-amino-3-methyl-3-sulfinylbutyric acid (sulbactam penicillamine). Background technique [0002] (2S) The structural formula of 2-amino-3-methyl-3-sulfinylbutyric acid (sulbactam penicillamine) is [0003] [0004] Sulbactam sodium is a semi-synthetic β-lactam inhibitor, which has a strong irreversible competitive inhibitory effect on β-lactamase produced by Staphylococcus aureus and most gram-negative bacteria. Therefore, it is increasingly used in combination with penicillin or cephalosporin drugs, which has a good antibacterial synergistic effect. In order to control the quality of its products, the Chinese Pharmacopoeia (CP) 2010 edition, United States Pharmacopoeia (USP) 34 edition, Japanese Pharmacopoeia (JP) 16 edition, European Pharmacopoeia (EP) 7.0 edition, European Pharmacopoeia (BP) 2011 edition all included them Quality Standard. [0005] During the inspection of product q...

Claims

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Application Information

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IPC IPC(8): C07C313/04
Inventor 柴建华刘亚林许蓓珍
Owner JIANGXI FUSHINE PHARMA CO LTD
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