Synthetic process for compound D-2-aminoxy-3-methylbutyric acid

A technology of methyl butyric acid and D-2-, which is applied in the field of synthesis technology of compound D-2-aminooxy-3-methyl butyric acid, can solve the problems of complex production process, low production efficiency and high cost. , to achieve the effect of overcoming many processes, improving productivity and improving work efficiency

Inactive Publication Date: 2016-06-01
QINGDAO SHOUTAI AGRI SCI & TECH CO LTD
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Problems solved by technology

In the synthetic process method of D-2-aminooxy-3-methylbutyric acid at present, technological process is not easy to implement, and the product purity of generation is low, and reaction condition is harsh, and reactant one-way conversion rate is low, and manufacturing procedure is complicated, Low production efficiency and high cost, not suitable for mass production

Method used

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Effect test

Embodiment

[0015] The synthetic technique of compound D-2-aminooxy-3-methylbutanoic acid of the present embodiment comprises the following steps:

[0016] (1) Using water as the medium, react L-valine with concentrated sulfuric acid and sodium nitrite to obtain compound (S)-2-hydroxy-3-methylbutanoic acid;

[0017] (2) Under the protection of argon, the compound (S)-2-hydroxy-3-methylbutyric acid was reacted with acetyl chloride to obtain the compound (S)-2-acetoxy-3-methylbutyric acid;

[0018] (3) Using dichloromethane as a solvent, DCC as a condensation agent, and DMAP as a catalyst, the compound (S)-2-acetoxy-3-methylbutyric acid is condensed with tert-butanol to obtain the compound (S) - tert-butyl 2-acetoxy-3-methylbutyrate;

[0019] (4) In a mixed solution of MeOH and water, compound (S)-2-acetoxy-3-methylbutyrate tert-butyl reacts with K2CO3 to obtain compound (S)-2-hydroxyl-3-methyl tert-butyl butyrate;

[0020] (5) With THF as solvent, diethyl azodicarboxylate (DEAD) and tri...

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Abstract

The invention discloses a synthetic process for a compound, i.e., D-2-aminoxy-3-methylbutyric acid. The synthetic process synthesizes non-natural D-2-aminoxy-3-methylbutyric acid with natural amino acid L-valine as a starting raw material through diazotization hydrolysis, acetyl protection, t-butyl esterification, deacetylation, Mitsunobu reaction, removal of a phthalyl group, hydrolysis of tert-butyl ester, etc. The synthetic process has the following advantages: raw materials are easily available and cheap; synthesis operation is simple; reaction conditions are mild and easy to control; reaction selectivity is good; yield is high; and the process is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis process of compound D-2-aminooxy-3-methylbutanoic acid. Background technique [0002] Methylbutyric acid is a food and feed additive, and is used as a raw material for blending strawberry, cheese, apricot, jackfruit, butter and other food flavors. In the synthetic process method of D-2-aminooxy-3-methylbutyric acid at present, technological process is not easy to implement, and the product purity of generation is low, and reaction condition is harsh, and reactant one-way conversion rate is low, and manufacturing procedure is complicated, The production efficiency is low and the cost is high, so it is not suitable for large-scale production. Contents of the invention [0003] In order to overcome the above-mentioned technical problems existing in the prior art field, the object of the present invention is to provide a synthesis process of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/20
Inventor 张晶
Owner QINGDAO SHOUTAI AGRI SCI & TECH CO LTD
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