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Method for preparing N-acetyl-DL-leucine

A technology of leucine and acetyl, which is applied in the field of amino acid preparation, can solve the problems of cumbersome preparation methods and high costs, and achieve the effects of reducing production steps, reducing emissions, and improving yields

Inactive Publication Date: 2015-05-06
宁波海硕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many kinds of amino acids, taking N-acetyl-DL-leucine as an example, the current preparation method of N-acetyl-DL-leucine is relatively cumbersome and the cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0013] Add 1000ML 2NNaOH to 100gL-leucine and heat up to dissolve, add 1ML salicylaldehyde, keep warm at 95°C for 3 hours, the measured optical rotation is 0, cool to 5°C and keep it, add 80ML acetic anhydride dropwise, keep it for 0.5 hours after the dropwise addition, Raise the temperature to 60 degrees, add an appropriate amount of activated carbon to decolorize, add 160ML HCl to adjust the pH to 2.5, cool to 4 degrees, suction filter, and dry 118g.

example 2

[0015] Add 1200ML 2NNaOH to 100gL-leucine and dissolve it, add 3ML salicylaldehyde, keep warm at 95°C for 3 hours, the measured optical rotation is 0, cool to 5°C and keep it, add 80ML acetic anhydride dropwise, keep it for 0.5 hours after the addition , heat up to 60 degrees, add an appropriate amount of activated carbon to decolorize, add 180ML HCl to adjust the pH to 3.0, cool to 4 degrees, filter with suction, and dry 110g.

example 3

[0017] Add 100gL-leucine to 1000ML 2NNaOH and heat up to dissolve, add 2ML salicylaldehyde, keep warm at 95°C for 3 hours, the measured optical rotation is 0, cool to 5°C and keep it, add 80ML acetic anhydride dropwise, keep it for 0.5 hours after the dropwise addition , heat up to 60 degrees, add an appropriate amount of activated carbon to decolorize, add 180ML HCl to adjust the pH to 3.0, cool to 4 degrees, suction filter, and dry 120g.

[0018] The invention provides an alkaline dissolving environment for leucine through lye, avoids the problem of difficult treatment after racemization under acetic acid conditions, reduces the discharge of acid gas, reduces the consumption of acetic anhydride, reduces costs, reduces production steps, and improves yield. Rate.

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PUM

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Abstract

The invention relates to a method for preparing N-acetyl-DL-leucine. The method comprises the following steps: adding a proper amount of L-leucine under an alkaline condition; adding a small amount of a catalyst for racemization and dropwise adding 1-1.5 mol of acetic anhydride for acetylation; adding hydrochloric acid to adjust the pH to 2.5; and freezing and crystallizing. The method provided by the invention provides a dissolving environment for leucine by virtue of alkali liquor, so that the problem of post-treatment of racemization is hard under the condition of acetic acid; and emission of acid gas is reduced, the use level of acetic anhydride is reduced, the cost is lowered, the production steps are reduced and the yield is improved.

Description

technical field [0001] The invention relates to a preparation method of amino acid, especially a preparation method of N-acetyl-DL-leucine. Background technique [0002] Amino acid is a general term for a class of organic compounds containing amino and carboxyl groups. The basic unit of biofunctional macromolecular protein is the basic substance that constitutes the protein required for animal nutrition. It is an organic compound containing a basic amino group and an acidic carboxyl group. There are many types of amino acids, taking N-acetyl-DL-leucine as an example, the current preparation method of N-acetyl-DL-leucine is relatively cumbersome and the cost is relatively high. Contents of the invention [0003] The purpose of the present invention is to solve the defects in the preparation method of N-acetyl-DL-leucine in the prior art, and provide a preparation method of N-acetyl-DL-leucine with simple steps and high synthesis efficiency. [0004] In order to achieve th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/47C07C231/02
Inventor 竺东海
Owner 宁波海硕生物科技有限公司