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Process for synthesizing an aminopropanol

A technology of aminopropanol and synthesis technology, applied in the field of synthesis technology of pharmaceutical intermediates, can solve the problems of only 12%, harsh reaction conditions, low yield and the like, and achieves the effects of easy operation and simple steps

Inactive Publication Date: 2013-04-03
李兰心
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conventional method is obtained by catalytic hydrogenation of β-hydroxypropionitrile, adding β-hydroxypropionitrile, Rainy nickel, ethanol, and ammonia into an autoclave for reaction, and the resulting 3-aminopropanol has a purity of more than 95% and a yield close to 60% %; In 2004, people such as Sylvie Picard utilized DMSO and dichloromethane to synthesize 3-aminopropanol, and the product purity obtained had 98%, but the yield only had 12%; In 2007, people such as Springgerta used 3-aminopropanol Ethyl acetate and 2-cyanoethanol are used to synthesize 3-aminopropanol, and high-purity products are also obtained, but the yield is still very low
The above-mentioned methods all have the disadvantages of dangerous raw materials, low yield, harsh reaction conditions, etc.

Method used

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  • Process for synthesizing an aminopropanol
  • Process for synthesizing an aminopropanol
  • Process for synthesizing an aminopropanol

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Experimental program
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Embodiment Construction

[0017] Processing step of the present invention is:

[0018] 1. Synthesis of Hydrazine

[0019] The reaction equation is:

[0020]

[0021] 2. Synthesis of Acyl Azides

[0022] The reaction equation is:

[0023]

[0024] 3. Synthesis of 3-aminopropanol

[0025] The reaction equation is:

[0026]

[0027] When preparing acyl azide, the reaction temperature must be controlled below 0°C. When the temperature is too high, the acyl azide formed is unstable and will decompose immediately. At the same time, other by-products will be formed, and the yield of the target product will be very low.

[0028] When preparing acyl azide, the reaction is carried out under acidic conditions, so it should be washed with saturated sodium bicarbonate solution to keep the product neutral, then washed with distilled water, and finally dried with anhydrous sodium sulfate. The hydrochloric acid added to prepare the acyl azide is dilute hydrochloric acid, and the pH is not easy to be too ...

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Abstract

The invention relates to a process for synthesizing a medicinal intermediate and particularly relates to a process for synthesizing an aminopropanol, which has the advantages of safe raw materials, high yield and mild reaction condition. According to the technical scheme of the invention, ring opening is carried out on 1,4-butyrolactone, serving as a raw material, under the action of hydrazine hydrate, the aqueous solution of sodium nitrite is added to generate acyl azide, and finally the rearranging is carried out to generate 3-aminopropanol.

Description

Technical field: [0001] The present invention relates to a kind of synthesis technology of medicine intermediate, more specifically, relate to a kind of synthesis technology of aminopropanol. Background technique: [0002] 3-Aminopropanol is a commonly used drug intermediate for the synthesis of drugs such as cyclophosphamide and propodin, and can also be used for the synthesis of DL-panthenol. The conventional method is obtained by catalytic hydrogenation of β-hydroxypropionitrile, adding β-hydroxypropionitrile, Rainy nickel, ethanol, and ammonia into an autoclave for reaction, and the resulting 3-aminopropanol has a purity of more than 95% and a yield close to 60% %; In 2004, people such as Sylvie Picard utilized DMSO and dichloromethane to synthesize 3-aminopropanol, and the product purity obtained had 98%, but the yield only had 12%; In 2007, people such as Springgerta used 3-aminopropanol Ethyl acetate and 2-cyanoethanol are used to synthesize 3-aminopropanol, and high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/08C07C213/02
Inventor 李兰心
Owner 李兰心
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