Method for synthesizing (S)-2-aminobutanol

A technology of aminobutyric acid and methylenebisacrylamide, which is applied in the field of synthesis of -2-aminobutanol, can solve problems such as inability to apply industrialized production, difficulty in obtaining raw materials, low yield and low efficiency, and the like, and achieve catalytic efficiency Improve, improve quality and yield, reduce the effect of by-products

Active Publication Date: 2016-04-13
JIANGXI XIANKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Raw materials used in such methods are difficult to obtain and expensive and rarely used
[0043] In addition, French patent FR2577242 uses electrochemical methods, German patent DE2446320 uses transaminase biological methods, etc. These methods are still in the research stage,

Method used

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  • Method for synthesizing (S)-2-aminobutanol
  • Method for synthesizing (S)-2-aminobutanol
  • Method for synthesizing (S)-2-aminobutanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] (1) Preparation of supported palladium catalyst

[0079] 100 parts by weight of acrylic acid (pretreated by distillation under reduced pressure), 10 parts by weight of water-soluble chitosan (deacetylation degree 90%, molecular weight is 3 * 10 5 , purchased from Zhejiang Golden Shell Pharmaceutical Co., Ltd.), 3 parts by weight of N,N-methylenebisacrylamide were dissolved in 1000mL deionized water, and ultrasonically oscillated to make the mixture uniform. Then, nitrogen gas was continuously introduced, and the temperature was raised to 60 ℃, under stirring, slowly add 1 part by weight of initiator (the initiator is potassium peroxodisulfate / sodium bisulfite with a molar ratio of 2:1), react for 2 hours to obtain a hydrogel, adjust the pH value to neutral Afterwards, it was washed with ethanol, dried at 50°C to constant weight and crushed to 80 mesh to obtain a catalyst carrier;

[0080] According to the ratio of the catalyst carrier to the palladium chloride aqueous ...

Embodiment 2～-5

[0091] (1) Preparation of supported palladium catalyst

[0092] Other steps are with embodiment 1, and difference only is the concentration and the consumption of palladium chloride aqueous solution, see following table 2:

[0093] Table 2: The different consumptions of palladium chloride in embodiment 2~5

[0094]

[0095] (2) Catalytic hydrogenation

[0096] Other steps are with embodiment 1, and difference only is that added catalyst type and consumption, catalyzer adopts the supported palladium catalyst prepared by the step (1) of above-mentioned embodiment 2~5 respectively, the content of palladium active component is the same in each embodiment. It is 0.1% of the weight of (S)-2-aminobutyric acid, based on which the amount of supported palladium catalyst used in each embodiment is calculated. Embodiment 1~5 hydrogenation reaction required time contrast, see following table 3:

[0097] Table 3: The time required for the hydrogenation reaction in Examples 1 to 5

[...

Embodiment 6

[0103] (1) Preparation of supported ruthenium catalyst

[0104] 100 parts by weight of acrylic acid (pretreated by distillation under reduced pressure), 10 parts by weight of water-soluble chitosan (deacetylation degree 90%, molecular weight is 3 * 10 5 , purchased from Zhejiang Golden Shell Pharmaceutical Co., Ltd.), 3 parts by weight of N,N-methylenebisacrylamide were dissolved in 1000mL deionized water, and ultrasonically oscillated to make the mixture uniform. Then, nitrogen gas was continuously introduced, and the temperature was raised to 60 ℃, under stirring, slowly add 1 part by weight of initiator (the initiator is potassium peroxodisulfate / sodium bisulfite with a molar ratio of 2:1), react for 2 hours to obtain a hydrogel, adjust the pH value to neutral Afterwards, it was washed with ethanol, dried at 50°C to constant weight and crushed to 80 mesh to obtain a catalyst carrier;

[0105] According to the ratio of the catalyst carrier to the ruthenium chloride aqueous ...

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Abstract

The invention provides a method for synthesizing (S)-2-aminobutanol. The method sequentially comprises steps as follows: (1) a supported metal catalyst is prepared; (2), (S)-2-aminobutanol is dissolved in deionized water, the pH (potential of hydrogen) value is adjusted to be 1-5, and the supported metal catalyst is added; hydrogen is introduced, the reaction temperature is controlled in the range from 60 DEG C to 70 DEG C, the reaction pressure is 2-4 MPa, and the mixture continuously reacts for 4-10 hours in the hydrogen atmosphere until hydrogen absorption stops; (3) after the reaction ends, the catalyst is separated from a reaction liquid, and a finished product (S)-2-aminobutanol is obtained through aftertreatment of filtrate. The method is low in production cost and simple and convenient to operate, raw materials are simple and easy to obtain, little pollution is caused to the environment, the operation is safety, the production yield is high, and the product quality is stable.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing (S)-2-aminobutanol used as a pharmaceutical intermediate. Background technique [0002] (S)-2-Aminobutanol is an important class of fine chemical intermediates, which can be used to prepare emulsifiers, surfactants, resinizers, polishing waxes, vulcanization accelerators, acid gas absorbents, etc. The product is the most critical intermediate of the anti-tuberculosis drug ethambutol hydrochloride. [0003] Ethambutol hydrochloride, as an anti-tuberculosis drug, is widely used in the treatment of various types of pulmonary tuberculosis and extrapulmonary tuberculosis. It has a market share of more than 13%, ranking fourth. It has a strong antibacterial effect on various mycobacteria such as Mycobacterium bovis and Human Mycobacterium. Mycobacterium tuberculosis has no cross-resistance between ethambutol hydrochloride and other anti-tuberculosis drugs. T...

Claims

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Application Information

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IPC IPC(8): C07C215/08C07C213/00B01J27/13
CPCB01J27/13C07C213/00C07C213/10C07C215/08
Inventor 周火平周晓军李石钟
Owner JIANGXI XIANKANG PHARMA CO LTD
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