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3-amino propanesulfonic acid preparation method

A technology of aminopropanesulfonic acid and sodium sulfate, which is applied in the intermediate of calcium acamprosate and the new preparation field of 3-aminopropanesulfonic acid, can solve the problems of high raw material price and high production cost, and achieve low production cost, The effect of low cost and simple operation

Active Publication Date: 2009-02-11
HANGZHOU FST PHARMA
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Problems solved by technology

[0008] The above two patents apply for high production raw material prices, resulting in high production costs

Method used

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Embodiment 1

[0023] Example 1. Dissolve 1 mol of sodium sulfite in 0.3 L of water, add 1 mol of acrylonitrile and 0.5 mol of 98% concentrated sulfuric acid dropwise at room temperature at the same time, and dropwise add in about 1 hour. After the reaction is complete, set the pH value of the system to 7, and distill to dryness under negative pressure. Obtain 3-sulfopropionitrile and sodium sulfate solids; cool to 30°C, add 0.8L of absolute ethanol to dissolve the solids, heat up to 78°C and reflux for 2 hours, filter while hot to remove sodium sulfate; place the filtrate in a hydrogenation reactor, Add ammonia ethanol solution, set the pH value of the system to 10, use Raney nickel as the catalyst, the addition amount is 2% of the total amount of the reaction system, hydrogenation reaction, keep the reaction temperature at 60°C, the pressure at 2.0MPa, and the time for 6h, Until no hydrogen is absorbed; after the reaction, ethanol is recovered, and the material is cooled and precipitated t...

Embodiment 2-3

[0026]

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Abstract

The invention relates to a new preparation method of 3-aminopropanesulfonic acid, which is required for solving the problem that a new preparation method has raw materials with comparatively low prices and is more applicable to industrialized production. The method includes the steps as follows: 1) sodium sulfite is dissolved in water and acrylonitrile and sulphuric acid are added at room temperature in a dropwise manner. After the dropwise operation, the pH value of the system is set as 6 to 7 and the system is distilled under negative pressure until no water is available, so as to obtain 3-sulfo-ethyl cyanide and sodium sulfate solid; 2) absolute ethanol is added for dissolving the 3-sulfo-ethyl cyanide and the sodium sulfate solid, and then heated up for reflux, well stirred and filtered while hot; sodium sulfate is removed and ethanol filtrate is moved to a hydrogenation reaction kettle and cholamine solution is added to set the pH value of the system as 9 to 10, and then Raney nickel in catalysis amount and hydrogen gas are added for full hydrogenation. A catalyst is filtered and the ethanol is recycled by distilling, and then the 3-aminopropanesulfonic acid is obtained by filtering after cooling.

Description

technical field [0001] The invention relates to the technical field of organic compounds, in particular to a new preparation method of 3-aminopropanesulfonic acid, an intermediate of calcium acamprosate. Background technique [0002] Alcohol abuse and alcohol dependence are the third public health problems after cardiovascular diseases and tumors. It is estimated that about 20% of the people in the United States have had alcohol abuse or alcohol dependence, and there are 15.4 million people with serious alcohol-related problems, and the life expectancy reduction caused by alcoholism is greater than that of cardiovascular disease. Be obvious. In 1992, my country's Alcohol Dependence Collaborative Research Group used unified tools and diagnostic criteria to conduct a systematic study on alcohol abuse and alcohol dependence in my country. As a result, among the 44,920 people investigated, 1,674 were clinically determined to be alcohol-dependent cases, and the average patient T...

Claims

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Application Information

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IPC IPC(8): C07C309/14C07C303/06C07C303/22
Inventor 凌建红徐伟
Owner HANGZHOU FST PHARMA
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