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D-aspartic acid derivative and preparation method thereof

A technology of aspartic acid and derivatives, applied in the field of D-aspartic acid derivatives and their preparation, can solve the problems of many side reactions, long reaction time, low yield and the like

Inactive Publication Date: 2019-11-05
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problems of long reaction time, many side reactions and low yield in the current preparation method of D-aspartic acid derivatives, the present invention provides a preparation method of D-aspartic acid derivatives

Method used

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  • D-aspartic acid derivative and preparation method thereof
  • D-aspartic acid derivative and preparation method thereof
  • D-aspartic acid derivative and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] This example provides a preparation method of D-aspartic acid derivatives.

[0022] Specifically include the following steps:

[0023] 1. Preparation of D-Aspartic Acid

[0024] Dissolve DL-aspartic acid at a concentration of 13.3g / L (0.1-4M) in water at 20°C, and control the pH range from 2.0 to 12.0, and cells containing L-aspartic acid-α-decarboxylase (detection activity meets every gram per hour> 120 μ mol) drop in the substrate, the addition amount of L-aspartic acid-alpha-decarboxylase is 1 / 2 of the substrate, heat preservation reaction is transformed completely to the substrate, and the gained material is liquid-solid After liquid separation, acid was added to adjust the pH of the obtained filtrate to 2.8-2.9, and the temperature was maintained at 48-50°C, and white crystals were precipitated from the filtrate. Filter after 30 minutes, wash the obtained white crystals with 0.2 times the volume of water, and vacuum dry at 100-120°C to obtain the finished product...

Embodiment 2

[0030] This example provides a preparation method of D-aspartic acid derivatives.

[0031] Specifically include the following steps:

[0032] 1. Preparation of D-Aspartic Acid

[0033] DL-aspartic acid with a concentration of 133g / L (1M) was dissolved in water at 40°C, and the pH range was controlled within 2.0 to 12.0, and the cell extract containing L-aspartic acid-α-decarboxylase ( The detected activity conforms to the per hour per gram > 120 μmol) into the substrate, the amount of L-aspartic acid-α-decarboxylase added is 1 / 3 of the substrate, and the reaction is incubated until the substrate is completely converted, and the obtained material is liquid-solid-liquid After separation, acid was added to adjust the pH of the resulting filtrate to 2.9-3.0, and the temperature was maintained at 46-48°C, and white crystals were precipitated from the filtrate. After 30 minutes, filter, wash the obtained white crystals with 0.5 times the volume of water, and vacuum-dry at 80-100°C...

Embodiment 3

[0039] This example provides a preparation method of D-aspartic acid derivatives.

[0040] Specifically include the following steps:

[0041] 1. Preparation of D-Aspartic Acid

[0042] Dissolve DL-aspartic acid hydrochloride with a concentration of 266g / L (2M) in water at 50°C, and control the pH range from 2.0 to 12.0, and the cells containing L-aspartic acid-α-decarboxylase and its extract (detection activity conforms to >120 μmol per hour per gram) into the substrate, the amount of L-aspartic acid-α-decarboxylase added is 1 / 5 of the substrate, and the reaction is incubated until the substrate is completely converted. After the solid-liquid separation of the obtained material and liquid, acid is added to adjust the pH of the obtained filtrate to 2.8-2.9, and the temperature is maintained at 44-56° C., and white crystals are precipitated from the filtrate. Filter after 30 minutes, wash the obtained white crystals with 1 volume of water, and vacuum dry at 60-80°C to obtain t...

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Abstract

The invention relates to the technical field of pharmacy, in particular to a preparation method of a D-aspartic acid derivative. The derivative is formed by a reaction of D-aspartic acid and liquid monohydric alcohol or organic acid. The reaction condition is simple, scale production is easy to achieve, the reaction time can be shortened significantly, the conversion rate can be 96% or above, there are few impurities in the reaction products, and the purity can reach 95% or above.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a D-aspartic acid derivative and a preparation method thereof. Background technique [0002] Amino acids are the basic constituent units of macromolecular proteins required for animal nutrition, and are classified according to the different side chain groups R. Among them, glutamic acid, arginine, aspartic acid, cystine, L-dopa and other amino acids can be used to improve muscle vitality, supplement nutrition and detoxification, etc., and can also be used alone for the treatment or auxiliary treatment of diseases, such as liver disease, gastrointestinal disease, encephalopathy, cardiovascular disease, respiratory disease, etc. Among them, aspartic acid has optical activity, that is, L amino type and D amino type. D-Aspartic acid is an important chiral compound, which plays an important role in medicine, food, etc., and can be used as a precursor and intermediate fo...

Claims

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Application Information

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IPC IPC(8): C07C227/16C07C227/34C07C229/24C12P13/20C12P41/00
CPCC07C227/16C07C227/34C12P13/20C12P41/00C07B2200/07C07C229/24
Inventor 曹珊何连顺李斌水
Owner JING JING PHARMA
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