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Resolution process of racemic amino pentanamide

A technology of racemic aminovaleramide and aminovaleramide, which is applied in the field of splitting technology of racemic aminovaleramide, can solve the problems of increasing waste discharge, low splitting yield, etc., and achieves the effect of improving splitting yield

Inactive Publication Date: 2012-12-19
ZHEJIANG BANGCHENG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Currently in the production of L-norvaline, in the resolution process of racemic aminovaleramide, methanol is used as solvent, not only the resolution yield is low, but also the amount of waste is increased

Method used

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  • Resolution process of racemic amino pentanamide

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Experimental program
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Effect test

Embodiment Construction

[0006] The present invention will be further described below in conjunction with specific examples.

[0007] 1. Embodiment

[0008] 1. Mix 105g of methanol and 45g of ethyl acetate to prepare a mixed solvent (the mass ratio of methanol and ethyl acetate should be kept at 1:2~2.5).

[0009] 2. Dissolve 20g of L-tartaric acid in 150g of the above-mentioned mixed solvent (wherein, the mass ratio of L-tartaric acid methanol to the above-mentioned mixed solvent should be kept at 1:7.5-8).

[0010] 3. Cool down to below 10°C, slowly add 40g of racemic aminovaleramide (the mass ratio of racemic aminovaleramide to the above L-tartaric acid should be kept at 2-2.5:1), and continue the reaction after adding After 2 to 2.5 hours, the discharge is filtered, and the filter cake is the resolution product L-aminovaleramide tartrate, and the weight of the wet product is 34.8g.

[0011] 2. Experimental data and results comparison

[0012]

[0013] As can be seen from the above table, whe...

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Abstract

The invention relates to a resolution process of racemic amino pentanamide, which comprises the following steps that methanol and ethyl acetate are prepared into a solvent mixture according to a mass ratio of 1:2 to 2.5, and then L-tartaric acid is dissolved into the solvent mixture according to a mass ratio of 1:1 7. 5 to 8; the temperature is reduced to below 10 DEG C, and the racemic amino pentanamide is slowly added according to a mass ratio of racemic amino pentanamide to L-tartaric acid of 2 to 2.5:1; and after addition, the reaction is continuously carried out for 2 to 2.5 hours, a material is discharged and filtered to obtain a filter cake which is the resolution product L-amino pentanamide tartrate. With the resolution process, the experimental data shows that the resolution rate can be increased by 15%.

Description

technical field [0001] The invention relates to a separation process of racemic aminovaleramide, in particular to the production of L-norvaline. Background technique [0002] Currently in the production of L-norvaline, in the separation process of racemic aminovaleramide, because methanol is used as solvent, not only the separation yield is low, but also the discharge of waste is increased. Contents of the invention [0003] The object of the present invention is to provide a kind of resolution process of racemic aminovaleramide that can improve resolution yield. [0004] The technical solution adopted by the present invention is: a splitting process of racemic aminovaleramide, which is characterized in that methanol and ethyl acetate are made into a mixed solvent at a mass ratio of 1:2 to 2.5, and then L-tartaric acid is 1: Dissolve in the above mixed solvent at a mass ratio of 7.5 to 8, then lower the temperature to below 10°C, and slowly add racemic aminopentanamide to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/06C07C231/20
Inventor 戚文萍邱辉强郑东有
Owner ZHEJIANG BANGCHENG CHEM
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