Preparation method of D-p-chlorophenylalanine

A technology of p-chlorophenylalanine and hydrochloric acid is applied in the field of preparation of D-p-chlorophenylalanine, can solve the problems of large reaction volume, increased concentration cost, low solubility and the like, and achieves low cost, simple method, high yield effect

Inactive Publication Date: 2016-07-13
郁庆明
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AI Technical Summary

Problems solved by technology

For some aromatic amino acids with large side chains and poor solubility, the reaction volume is large d

Method used

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Embodiment Construction

[0015] A preparation method of D-p-chlorophenylalanine, the method comprises the steps:

[0016] 1. Synthesis of acetylated D, L-p-chlorophenylalanine:

[0017] D,L-p-Chlorophenylalanine, dissolved in water, adjusted pH to 10 with alkali, temperature controlled at 0-5°C, acetic anhydride was added dropwise, pH was controlled with 5N sodium hydroxide during the reaction, and indene was used in the reaction solution The triketone develops color until the amino acid no longer develops color, indicating that all the amino acids are acetylated. Add hydrochloric acid to adjust the pH to 1-2, and a large amount of precipitated product appears. The crystals are collected by filtration, washed with acid water, and dried. The yield is 90%.

[0018] 2. Dissolve the acetylated D,L-p-chlorophenylalanine at 80°C, the concentration can reach 0.7M, add purified L-high temperature acylase, react for 48 hours, and separate by liquid phase detection The degree of deacetylation of D-p-chlorophe...

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Abstract

The invention relates to a preparation method of D-p-chlorophenylalanine. The method comprises the following steps: 1, dissolving D,L-p-chlorophenylalanine in water, adjusting the pH value to 10 with alkali, controlling the temperature in a range of 0-5 DEG C, dropwise adding acetic anhydride for a reaction, controlling the pH value with a 5N sodium hydroxide solution during the reaction, performing color development of a reaction solution with ninhydrin till amino acid is no longer subjected to color development, adjusting the pH value to 1-2 with hydrochloric acid, allowing a precipitation product to appear, performing filtering to collect a crystal, washing the crystal with an acid solution, and performing drying; 2, dissolving the obtained acetylated D,L-p-chlorophenylalanine at 80 DEG C, adding purified high-temperature-resistant L-acylase, performing a reaction for 48 h, detecting the separation degree through liquid-phase detection, performing cooling, adding hydrochloric acid to adjust the pH value to 1-2, allowing a precipitation product to appear, and performing filtering to obtain acetylated D-p-chlorophenylalanine; and 3, hydrolyzing the obtained acetylated D-p-chlorophenylalanine precipitation product with a 6N hydrochloric acid solution overnight to obtain D-p-chlorophenylalanine, and performing recrystallization. The method is low in cost and high in yield, and is simple.

Description

technical field [0001] The invention relates to a preparation method of D-p-chlorophenylalanine. Background technique [0002] Currently, the commonly used amidases in industry cannot withstand high temperature for a long time, and the splitting temperature is generally 37 degrees to achieve the highest efficiency of the enzyme. For some amino acids with poor solubility in aromatic and large side chains, due to low solubility, the reaction volume is large, which leads to an increase in industrial concentration costs and a low recovery yield. SUMMARY OF THE INVENTION [0003] The object of the present invention is to overcome above-mentioned deficiency, and a kind of preparation method of D-p-chlorophenylalanine with low cost, high yield and simple method is provided. [0004] The object of the present invention is achieved in this way: [0005] A preparation method of D-p-chlorophenylalanine, the method comprises the steps: [0006] 1. Synthesis of acetylated D, L-p-chl...

Claims

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Application Information

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IPC IPC(8): C12P41/00C12P13/22
Inventor 郁庆明
Owner 郁庆明
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