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Amino acid propylene ester hydrochloride and its preparation process

A technology of propylene ester hydrochloride and preparation process, applied in the direction of organic chemistry, etc., can solve the problems of residual impurities and inability to effectively remove impurities, and achieve the effect of improving yield and purity

Active Publication Date: 2021-08-24
NANJING REDWOOD FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Amino acid allyl ester hydrochloride is one of amino acid derivatives, which has a wide range of uses. In the prior art, there is an esterification reaction to form amino acid allyl ester hydrochloride, especially the use of thionyl chloride Esterification, but when thionyl chloride is esterified to form amino acid allyl ester hydrochloride, impurities remain. In the prior art, the post-treatment after the reaction is generally concentrated and directly crystallized. This post-treatment cannot effectively remove impurities. , so that the final product formed still contains a large amount of impurities

Method used

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  • Amino acid propylene ester hydrochloride and its preparation process
  • Amino acid propylene ester hydrochloride and its preparation process

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Embodiment 1

[0058] The present embodiment provides a preparation process of L-tryptophan allyl ester hydrochloride, comprising the following steps:

[0059] 24.7 g (0.121 mol) of L-tryptophan was weighed and mixed with 150 g of allyl alcohol, then the reaction solution was cooled to 0° C., and 28.8 g (0.242 mol) of thionyl chloride was added dropwise. The temperature control during the dropwise addition should not exceed 10°C.

[0060] After dripping, the temperature of the reaction solution was raised to 70 °C for 12 h, and the liquid phase was controlled.

[0061] The reaction was completed, the reaction solution was concentrated to obtain a concentrated solution, 200 mL of 15% sodium carbonate aqueous solution and 200 g of ethyl acetate were added to the concentrated solution, stirred at 25 ° C for 30 min, the organic layer was separated, the organic layer was dried over anhydrous sodium sulfate, and HCl / ethyl acetate was added dropwise. The PH of the ester was adjusted to 1, and the ...

Embodiment 2-4

[0063] Embodiment 2-4 provides a kind of preparation technology of L-tryptophan allyl ester hydrochloride, and its operation steps are the same as the preparation technology of L-tryptophan allyl ester hydrochloride provided in embodiment 1, and the difference lies in the specific operation Conditions vary. The specific table is as follows:

[0064]

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Abstract

The invention relates to the technical field of chemical synthesis, in particular to amino acid propylene ester hydrochloride and a preparation process thereof. The preparation steps of amino acid propylene ester hydrochloride include: extracting the reaction system formed after the esterification reaction of thionyl chloride, amino acid and allyl alcohol, and then crystallizing the organic layer formed by the extraction. The preparation process improves the post-treatment process after the reaction, can significantly remove unreacted raw materials in the reaction system after the reaction, and improves the yield and purity of the product.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to amino acid propylene ester hydrochloride and a preparation process thereof. Background technique [0002] Amino acid allyl ester hydrochloride is a kind of amino acid derivatives, and it has a wider range of uses, and in the prior art, the use of esterification to form amino acid allyl ester hydrochloride, especially the use of thionyl chloride Esterification is carried out, but when thionyl chloride is esterified to form amino acid allyl ester hydrochloride, there are impurities remaining, and in the prior art, the post-processing after the reaction is generally concentrated and directly crystallized, and the post-processing cannot effectively remove impurities. , so that the final product formed still contains a large amount of impurities. [0003] In view of this, the present invention is proposed. SUMMARY OF THE INVENTION [0004] The object of the present inve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/20
CPCC07D209/20
Inventor 吴法浩李钢高仰哲王志航
Owner NANJING REDWOOD FINE CHEM CO LTD