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A kind of preparation method of 3-aminobutanamide and/or 3-hydroxybutanamide

A technology of hydroxybutyramide and aminobutyramide, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of lack and unscaled industrial production, and achieves low production cost and raw material utilization. High efficiency, simple and efficient process

Active Publication Date: 2022-07-22
北京汇康博源医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is currently a lack of efficient process technology for the synthesis of these two C4 amides, resulting in the large-scale industrial production of these two typical C4 amides

Method used

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  • A kind of preparation method of 3-aminobutanamide and/or 3-hydroxybutanamide

Examples

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Embodiment 1

[0031] A preparation method of 3-aminobutanamide and / or 3-hydroxybutanamide, comprising the following steps:

[0032] (1) put the cold water (10 ℃) of 6g poly-3-hydroxybutyrate pure product, 20g into 100ml airtight reactor, control reactor temperature constant temperature at 10 ℃ by solvent bath, then pass through the reactor Enter ammonia gas, and make the ammonia gas pressure in the reactor reach 0.6MPa;

[0033] (2) Turn on the mechanical stirring and control the stirring speed to be 500 RPM, then heat up to 60 °C at a heating rate of 6 °C / min, and then react at 60 °C for 24h;

[0034] (3) cooling to room temperature after completion of the reaction, discharging and collecting residual ammonia, and collecting to obtain a clear and transparent liquid product. Qualitative and quantitative analysis by GCMS (see figure 1 ), the liquid product contains 2.1g of 3-aminobutanamide, 2.9g of 3-hydroxybutyramide and 0.8g of 3-aminobutyric acid (by-product), wherein 3-aminobutanamide...

Embodiment 2

[0036] A preparation method of 3-aminobutanamide and / or 3-hydroxybutanamide, comprising the following steps:

[0037] (1) put the cold water (1 ℃) of 6g poly-3-hydroxybutyrate pure product, 15g into 100ml airtight reactor, control reactor temperature constant temperature at 1 ℃ by solvent bath, then pass through the reactor Enter ammonia gas, and make the ammonia gas pressure in the reactor reach 0.6MPa;

[0038] (2) Turn on the mechanical stirring and control the stirring speed to be 300RPM, then heat up to 50°C at a heating rate of 6°C / min, and then react at 50°C for 48h;

[0039] (3) cooling to room temperature after completion of the reaction, discharging and collecting residual ammonia, and collecting to obtain a clear and transparent liquid product. After qualitative and quantitative analysis by GCMS, the liquid product contained 4.1g of 3-aminobutyramide, 1.1g of 3-hydroxybutyramide and 0.9g of 3-aminobutyric acid (by-product), among which, 3-aminobutanamide and 3 - T...

Embodiment 3

[0041] A preparation method of 3-aminobutanamide and / or 3-hydroxybutanamide, comprising the following steps:

[0042] (1) put the cold water (20 ℃) ​​of 6g poly-3-hydroxybutyrate pure product, 30g into 100ml airtight reactor, control reactor temperature constant temperature at 20 ℃ by solvent bath, then pass through the reactor Enter ammonia gas, and make the ammonia gas pressure in the reactor reach 1.2MPa;

[0043] (2) Turn on the mechanical stirring and control the stirring speed to be 100RPM, then heat up to 80°C at a heating rate of 6°C / min, and then react at 80°C for 3h;

[0044](3) cooling to room temperature after completion of the reaction, discharging and collecting residual ammonia, and collecting to obtain a clear and transparent liquid product. After qualitative and quantitative analysis by GCMS, the liquid product contained 3.8 g of 3-aminobutyramide, 1.3 g of 3-hydroxybutyramide and 0.7 g of 3-aminobutyric acid (by-product). The liquid product can be further r...

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Abstract

The invention relates to the technical field of C4 amide compounds, and specifically discloses a preparation method of 3-aminobutyramide and / or 3-hydroxybutyramide, which is characterized in that, comprising the following steps: (1) preparing poly-3-hydroxybutyrate And / or its copolymer and low-temperature polar solvent are put into the closed reactor, and the temperature of the reactor is controlled at a constant temperature of 1 to 20 ° C, then ammonia gas is introduced into the reactor, and the ammonia pressure in the reactor is reached. 0.2~1.2MPa; (2) be heated to 25~80 ℃ under stirring condition, then react at this temperature for 3~72h; (3) after the reaction is completed, cool down to room temperature, collect and obtain 3-aminobutanamide and 3-hydroxyl Liquid product of butanamide. The invention directly obtains high-value chemicals 3-aminobutyramide and 3-hydroxybutyramide through one-step reaction, the technological process is simple and efficient, and the production cost is low, which is beneficial to the large-scale industrial production of 3-aminobutanamide and 3-hydroxybutyramide , the total yield of 3-aminobutyramide and 3-hydroxybutyramide can reach 87%, and the raw material utilization rate is high.

Description

technical field [0001] The present invention relates to the technical field of C4 amide compounds, in particular to a preparation method of 3-aminobutanamide and / or 3-hydroxybutanamide. Background technique [0002] Amide compounds can be regarded as either nitrogen-containing derivatives of carboxylic acids or derivatives of ammonia or amines, so they have a wide range of application values. Aminobutyramide and hydroxybutyramide are two important C4 amide compounds, which have important potential applications in the fields of pharmaceutical intermediates, food, medicine and fine organic synthesis. Such as aminobutanamide compounds are widely used in the synthesis of antiepileptic drugs, anticonvulsants and other drugs. Hydroxybutyramide compounds are important raw materials for antithrombotic, antidiabetic and other medicines. In recent years, with the expansion of the application field of amide compounds and the development of downstream products, the demand for hydroxyb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/02C07C237/06C07C235/06
CPCC07C231/02C07C237/06C07C235/06
Inventor 康世民陈如洁姚家伟伍文峰张佳翔陈周华林佩敏朱钻楠
Owner 北京汇康博源医药科技有限公司