Preparation method of 3-aminopropanol

A technology of aminopropanol and benzyloxypropionitrile, which is applied in the field of preparation of 3-aminopropanol, can solve the problems of expensive starting materials, unfriendly environment, complex process, etc., and meet the requirements of high atom utilization and equipment requirements The effect of low cost and simple operation process

Active Publication Date: 2020-04-24
SHANDONG NHU FINE CHEM SCI & TECH CO LTD +2
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Problems solved by technology

[0007] Based on technical problems such as expensive starting materials, high toxicity, complex process, low yield, and environmental unfriendliness in the above-mentioned traditional 3-aminopropanol preparation method, the present The invention provides a new method for preparing 3-aminopropanol

Method used

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preparation example Construction

[0026] The embodiment of the present invention provides a kind of preparation method of 3-amino propanol, comprises the following steps:

[0027] (1) reacting acrylonitrile and benzyl alcohol under the catalysis of an alkali catalyst, and separating and obtaining 3-benzyloxypropionitrile from the resulting reaction solution;

[0028] (2) In a liquid-phase reaction system in which a hydrogenation catalyst exists, the 3-benzyloxypropionitrile is subjected to a hydrogenation reaction, and 3-aminopropanol is obtained by separating from the resulting reaction liquid.

[0029] The preparation method of 3-aminopropanol provided in the embodiment of the present invention adopts benzyl alcohol instead of water in the traditional acrylonitrile method for addition reaction, and can obtain the intermediate 3-benzyloxypropionitrile with high yield, almost no side effects The reaction takes place, and the product of the addition reaction is extracted and separated and can be used as a raw m...

Embodiment 1

[0041] (1) 53g of acrylonitrile and 119g of benzyl alcohol were added to the reaction kettle (the molar ratio of feed was 1.0:1.10), and 100mL of sodium hydroxide aqueous solution with a mass fraction of 25% was added, and after 2 hours of insulated reaction at 35°C, the reaction The liquid was extracted three times with toluene (3×100 mL), and the organic phase was collected and concentrated under reduced pressure to obtain the crude product of 3-benzyloxypropionitrile, and the yield of the crude product was 98.4%.

[0042] (2) the above-mentioned 3-benzyloxypropionitrile crude product is added in the autoclave, add Pd / C catalyst (add-on is 6wt% of 3-benzyloxypropionitrile crude product quality), add dichloromethane and water Mixed solvent 120mL (volume ratio 4:1). Cover the kettle lid, first replace the air in the kettle with nitrogen three times, then replace it once with hydrogen and pressurize to 0.45MPa, keep the reaction at 40°C for 4 hours, then carry out suction filtr...

Embodiment 2

[0044] (1) 53g of acrylonitrile and 113g of benzyl alcohol are added to the reactor (the molar ratio of feeding is 1.0:1.05), and 100mL of sodium hydroxide aqueous solution with a mass fraction of 30% is added, and after 2 hours of insulated reaction at 40°C, the reaction The liquid was extracted three times with toluene (3×100 mL), the organic phase was collected, and the organic phase was concentrated under reduced pressure to obtain a crude product of 3-benzyloxypropionitrile, and the yield of the crude product was 97.6%.

[0045] (2) the above-mentioned 3-benzyloxypropionitrile crude product is added in the autoclave, add Pd / C catalyst (add-on is 7wt% of 3-benzyloxypropionitrile crude product quality), add dichloromethane and water Mixed solvent 120mL (volume ratio 5:1). Cover the kettle lid, first replace the air in the kettle with nitrogen three times, then replace it with hydrogen once and pressurize to 0.5MPa. After the reaction at 45°C for 4 hours, the reaction soluti...

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Abstract

The invention relates to a preparation method of 3-aminopropanol, wherein the preparation method comprises the following steps: (1) carrying out a reaction on acrylonitrile with benzyl alcohol under the catalysis of a base catalyst, and separating the obtained reaction solution to obtain 3-benzyloxypropionitrile; and (2) in a liquid-phase reaction system in the presence of a hydrogenation catalyst, carrying out a hydrogenation reaction on the 3-benzyloxypropionitrile, separating the obtained reaction liquid to obtain 3-aminopropanol, and recycling the obtained by-product toluene as an extractant in the step (1).

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 3-aminopropanol. Background technique [0002] 3-Aminopropanol is a commonly used drug intermediate, which is used to synthesize D-panthenol, cyclophosphamide, Xanthodin and other drugs. Among them, D-panthenol is an excellent skin and hair protectant, which can keep the skin soft and the hair shiny and oily. It is widely used in hair care products and cosmetics, and can also be used in medicine, health food and other fields. Cyclophosphamide is an alkylating agent, which is mainly used for tumor immunity. It has obvious inhibitory effect on a variety of tumors, and has great effects on different systemic necrotic vasculitis, dermatomyositis, polymyositis, and scleroderma. Strong indication. Xinkeding is a calcium antagonist drug that inhibits Ca 2+ Transported into cells, thereby inhibiting myocardial contractility, relaxing vascular smooth m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/08
CPCC07C253/30C07C213/00C07C255/16C07C215/08
Inventor 李守垒李博王钰陈亚君
Owner SHANDONG NHU FINE CHEM SCI & TECH CO LTD
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