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Method for preparing aminoacetaldehyde dialkyl acetal

A technology of aminoacetaldehyde dialkyl alcohols and low-carbon alcohols, which is applied in chemical instruments and methods, the preparation of organic compounds, and the preparation of aminohydroxyl compounds, etc., and can solve the problems of unfavorable industrial production, large amount of "three wastes" and large consumption Energy consumption and other issues, to achieve significant application value, simplified operation, less dangerous effect

Inactive Publication Date: 2021-10-08
厦门优孚利生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This traditional process route is a method commonly used in industrial production at home and abroad. Although the process is mature and the raw materials are easy to obtain, the amount of "three wastes" is relatively large and the yield is low, which is not conducive to industrial production.
In addition, excessive ammonia water is required in the reaction of the traditional process route, so that the PH value must be adjusted with lye, resulting in the need to distill a large amount of water for post-treatment, consuming a large amount of energy and causing environmental problems.

Method used

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  • Method for preparing aminoacetaldehyde dialkyl acetal
  • Method for preparing aminoacetaldehyde dialkyl acetal
  • Method for preparing aminoacetaldehyde dialkyl acetal

Examples

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Embodiment 1

[0045] The method for preparing aminoacetaldehyde dimethyl acetal in this embodiment comprises the following steps:

[0046] 1) Preparation of formula III: Add benzylamine formula I (428g, 4mol) into the reaction flask, then add acid-binding agent potassium carbonate (276g, 2mol), heat up to 120-125°C, and control the temperature at 120-125°C, Start to slowly add formula II (R is methyl, 248g, 2mol) dropwise. After the dropwise addition, keep warm for 1-2 hours, cool down and suction filter, and the filtrate is distilled under reduced pressure to reclaim benzylamine to obtain the raffinate formula III (385g). Go to the next reaction.

[0047] 2) Preparation of aminoacetaldehyde dimethyl acetal: Add 1000ML of methanol, 50g of water, and ammonium formate (126g, 2mol) to the raffinate formula III obtained in the above steps, raise the temperature to 60-65°C, and raise the temperature of the palladium carbon fixed bed to 60-65°C, start the damping pump, adjust the flow rate to 20...

Embodiment 2

[0049] The method for preparing aminoacetaldehyde dimethyl acetal in this embodiment comprises the following steps:

[0050] 1) Preparation of formula III: add benzylamine formula I (856g, 8mol) into the reaction flask, then add acid-binding agent potassium carbonate (414g, 3mol), heat up to 120-140°C, and control the temperature at 120-140°C, Start to slowly add formula II (R is methyl, 248g, 2mol) dropwise. After the dropwise addition, keep warm for 1-2 hours, cool down and suction filter, and the filtrate is distilled under reduced pressure to reclaim benzylamine to obtain the raffinate formula III (385g). Go to the next reaction.

[0051]2) Preparation of aminoacetaldehyde dimethyl acetal: Add 1000ML of ethanol, 50g of water, and ammonium formate (252g, 4mol) to the raffinate formula III obtained in the above steps, raise the temperature to 60-80°C, and raise the temperature of the palladium carbon fixed bed to At 60-80°C, start the damping pump, adjust the flow rate to 2...

Embodiment 3

[0054] This embodiment prepares the method for aminoacetaldehyde diethyl acetal, comprises the following steps:

[0055] 1) Preparation of formula III: Add benzylamine formula I (428g, 4mol) into the reaction flask, then add acid-binding agent potassium carbonate (276g, 2mol), heat up to 120-125°C, and control the temperature at 120-125°C, Start to slowly drop formula II (R is ethyl, 266g, 2mol), after the dropwise addition is completed, keep warm for 1-2 hours, cool down and suction filter, and the filtrate is distilled under reduced pressure to reclaim benzylamine to obtain the raffinate formula III (440g), directly Go to the next reaction.

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Abstract

The invention discloses a method for preparing aminoacetaldehyde dialkyl acetal. The method comprises the following steps of: S1, subjecting raw materials of benzylamine shown as a formula I and a formula II to reacting under the action of an acid-binding agent to generate a substance as shown in a formula III; S2, adding low-carbon alcohol and an aqueous ammonium formate solution into the substance as shown in the formula III obtained in the step S1, conducting mixing, conveying the obtained mixture to a palladium-carbon fixed bed, and carrying out a catalytic reaction to obtain a substance as shown in a formula VI; and S3, transferring reaction liquid prepared in the step S2 to a rectifying tower, and conducting distilling to obtain a target product as shown in a formula VI. By adopting the method, the high-purity aminoacetaldehyde dialkyl acetal can be prepared, and the industrial production requirements of the aminoacetaldehyde dialkyl acetal can be met.

Description

technical field [0001] The invention relates to a method for preparing aminoacetaldehyde dialkyl acetal. Background technique [0002] Aminoacetaldehyde dialkyl acetal, such as aminoacetaldehyde dimethyl acetal and aminoacetaldehyde diethyl acetal, aminoacetaldehyde dimethyl acetal (C 4 h 12 NO 2 ), Aminoacetaldehyde dimethyl acetal, also known as aminoacetaldehyde dimethyl acetal, is a colorless liquid, often used as a pharmaceutical intermediate, such as in the effective synthesis of proline analogs from ascorbic acid through a 3-step reaction, and also used in Synthesized anti-AIDS raw material drug dolutegravir, anthelmintic drug praziquantel, etc. [0003] The structural formula of aminoacetaldehyde dialkyl acetal is as follows: [0004] [0005] The route that the traditional technique of preparing aminoacetaldehyde dialkyl alcohol takes is that chloroacetaldehyde dimethyl acetal or chloroacetaldehyde diethyl acetal (purity > 99%) and ammonia directly carry o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/40C07C213/08C07C213/10
CPCC07C213/02C07C213/08C07C213/10C07C217/40
Inventor 黄振辉林峰陶平
Owner 厦门优孚利生物医药科技有限公司
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