Synthesis method of ethyl 4-cyano-3-hydroxybutyrate

A technology of ethyl hydroxybutyrate and a synthesis method, which is applied in the direction of carboxylic acid nitrile purification/separation, organic chemistry, fermentation, etc., can solve the problems of large amount of extractant, large amount of sodium cyanide, and high operation cost, and achieves an increase in the The effect of technological advancement, environmental protection cost reduction, and mild reaction

Inactive Publication Date: 2020-11-03
LIANYUNGANG DIPU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) This synthetic route sodium cyanide consumption is big, and utilization rate is low, and molar ratio is 1.6-1.8 times of 4--chloro-3-hydroxybutyrate ethyl ester, produces a large amount of cyanide-containing waste water, and treatment cost is high;
[0007] (2) The synthetic route extractant uses a large amount, the number of extractions is many, and the operating cost is high;
[0008] (3) The reaction control of this synthetic route requires a pH value of 6.9±0.1, which requires high reaction control and high operating costs;

Method used

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  • Synthesis method of ethyl 4-cyano-3-hydroxybutyrate

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Embodiment 1

[0036] A kind of 4-cyano group-3-hydroxybutyrate ethyl ester synthetic method, comprises the following steps:

[0037] (1) Reaction synthesis: add 80ml of deionized water in the reaction flask, drop into 17.3g (0.1mol) of 4-chloro-3-hydroxybutyrate ethyl ester (purity 96%), add ammoniacal liquor (25%) to adjust pH6. 9-7.1, add 0.85g dehalogenase, then pass through hydrocyanic acid, and add ammonia water (25%) solution to adjust the pH to 6.9-7.1, control the temperature at 40-55°C, and react until the analysis of 4-chloro-3- The ethyl hydroxybutyrate content is ≤1%, and then spot the plate again to confirm that the reaction is complete, confirm the end point of the reaction, and obtain the reaction liquid;

[0038] (2) Precipitation and water removal: the reaction solution is concentrated and dehydrated, the temperature is controlled below 60°C, the vacuum is at 15Kpa, and concentrated to 35-45% of the volume of the feed liquid to obtain the feed liquid;

[0039] (3) Desaltin...

Embodiment 2

[0043] A kind of 4-cyano group-3-hydroxybutyrate ethyl ester synthetic method, comprises the following steps:

[0044] (1) Reaction synthesis: add 80ml of deionized water into the reaction flask, drop into 17.3g (0.1mol) of ethyl 4-chloro-3-hydroxybutyrate (purity 96%), add methylamine water (40%) solution Adjust the pH to 6.9-7.1, add 0.85g of dehalogenase, then pass through hydrocyanic acid, add methylammonia (40%) solution at the same time to adjust the pH to 6.9-7.1, control the temperature at 40-55°C, and react until the analysis of 4- The content of ethyl chloro-3-hydroxybutyrate is ≤1%, and then spot the plate again to confirm that the reaction is complete, confirm the end point of the reaction, and obtain the reaction solution;

[0045] (2) Precipitation and water removal: the reaction solution is concentrated and dehydrated, the temperature is controlled below 60°C, the vacuum is at 15Kpa, and each batch is concentrated to 35-45% of the volume of the feed liquid to ob...

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Abstract

The invention provides a synthesis method of ethyl 4-cyano-3-hydroxybutyrate, and relates to the technical field of ethyl butyrate synthesis. The synthesis method comprises the following steps: performing reaction synthesis: adding deionized water into a reaction flask, adding ethyl 4-chloro-3-hydroxybutyrate, adding a buffer agent to regulate the pH value to 6.9-7.1, adding dehalogenase, introducing hydrocyanic acid, adding the buffer agent again to regulate the pH value to 6.9-7.1, wherein the reaction temperature is 40-55 DEG C, performing reacting until the content of ethyl 4-chloro-3-hydroxybutyrate is analyzed to be less than or equal to 1%, then carrying out plate dotting again to confirm that the reaction is complete, and confirming a reaction end point to obtain a reaction solution; and then carrying out steps of desolvation and water removal, filtration and desalting, extraction and washing, and desolvation and rectification subsequentially. Compared with the prior art, the synthesis method has the advantages that the cost of links such as three-waste treatment, equipment investment and manual investment is reduced, and the technical advancement of the product is improved.

Description

technical field [0001] The invention relates to the technical field of ethyl butyrate synthesis, in particular to a synthesis method of ethyl 4-cyano-3-hydroxybutyrate. Background technique [0002] Ethyl 4-cyano-3-hydroxybutyrate is the key intermediate of atorvastatin. Atorvastatin is a selective inhibitor of HMG-CoA reductase, mainly used to reduce plasma cholesterol and lipoprotein levels, and can pass Increasing the level of low-density lipoprotein (LDL) on the surface of liver cells is a commonly used cardiovascular drug for regulating blood lipids. [0003] The synthetic technique of ethyl cyano-3-hydroxybutyrate is as follows at present: [0004] [0005] The disadvantages of the existing synthetic process route are as follows: [0006] (1) This synthetic route sodium cyanide consumption is big, and utilization rate is low, and molar proportion is 1.6-1.8 times of 4--chloro-3-hydroxybutyrate ethyl ester, produces a large amount of cyanide-containing waste water,...

Claims

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Application Information

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IPC IPC(8): C12P13/00C07C253/34C07C255/20
CPCC07C253/34C12P13/002C07C255/20
Inventor 孟明飞吴水亮靳洪欣
Owner LIANYUNGANG DIPU CHEM
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