Preparation method of L-p-chlorophenylalanine

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

Inactive Publication Date: 2016-07-13
郁庆明
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  • Application Information

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Problems solved by technology

For some aromatic amino acids with large side chains and poor solubility, the reaction volume is large due to low solubility, resulting in increased concentration costs and low recovery yields in the industry

Method used

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Embodiment Construction

[0013] A preparation method of L-p-chlorophenylalanine, said method comprising the steps of:

[0014] 1. Synthesis of acetylated D,L-p-chlorophenylalanine:

[0015] D, L-p-chlorophenylalanine, soluble in water, adjust the pH to 10 with alkali, control the temperature at 0-5°C, add acetic anhydride dropwise, use 5N sodium hydroxide to control the pH during the reaction, and use indene for the reaction solution Triketone develops color until the amino acid no longer develops color, indicating that all amino acids are acetylated. Add hydrochloric acid to adjust the pH to 1-2, and a large amount of precipitated products appear. The crystals are collected by filtration, washed with acid water, and dried. The yield is 90%.

[0016] 2. Dissolve acetylated D,L-p-chlorophenylalanine at 80°C, the concentration can reach 0.7M, add purified L-high temperature resistant acylase, react for 48 hours, and use liquid phase detection to resolve The degree of deacetylation of L-p-chlorophenyla...

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Abstract

The invention relates to a preparation method of L-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; and 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, filtering the acetylated D-p-chlorophenylalanine off with L-p-chlorophenylalanine left, and performing cation exchange for purification to obtain L-p-chlorophenylalanine. 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 L-p-chlorophenylalanine. Background technique [0002] The commonly used amidation enzymes in the industry cannot withstand high temperature for a long time, and the temperature for splitting is generally 37 degrees to achieve the highest efficiency of the enzyme. For some aromatic amino acids with large side chains and poor solubility, the reaction volume is relatively large due to low solubility, resulting in increased concentration costs and low recovery yields in industry. Contents of the invention [0003] The purpose of the present invention is to overcome above-mentioned deficiency, and a kind of preparation method of L-p-chlorophenylalanine with low cost, high yield and simple method is provided. [0004] The purpose of the present invention is achieved like this: [0005] A preparation method of L-p-chlorophenylalanine, said method comprising the steps of: [0006] 1. Synthesis of acetylate...

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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