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Preparation method of amino aminoacetaldehyde dimethyl acetal

A technology of aminoacetaldehyde dimethyl acetal and chloroacetaldehyde dimethyl acetal, which is applied in the field of medicine and chemical industry, can solve the problems of high cost, complex process, difficult promotion and industrialization, etc., and achieve the effect of improving recovery rate and purity

Inactive Publication Date: 2016-08-31
FUJIAN WANKE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing method for producing aminoacetaldehyde dimethyl acetal mainly uses vinyl acetate as the starting material, and produces the target product through processes such as bromination and synthesis, but the process is complicated, the cost is high, and it is not easy to popularize and industrialize

Method used

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  • Preparation method of amino aminoacetaldehyde dimethyl acetal

Examples

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Comparison scheme
Effect test

Embodiment 1

[0020] Add chloroacetaldehyde dimethyl acetal and methanol into the pressure reaction kettle, stir evenly; then add liquid ammonia, heat to 150°C and carry out high-pressure reaction; put the intermediate material into the concentration kettle, and carry out multiple distillations, the pressure of each distillation From high to low until methanol is successfully recovered, and the solution is centrifugally filtered; the concentration of 50% sodium hydroxide is added to the centrifuge to adjust the pH value to 12; rectification, extraction and dehydration are carried out under normal pressure And carry out secondary rectification again after purification, control secondary rectification as vacuum rectification to guarantee safety until collecting qualified cuts, obtain product product aminoacetaldehyde dimethyl acetal.

Embodiment 2

[0022] Add chloroacetaldehyde dimethyl acetal and methanol into the pressure reaction kettle, stir evenly; then add liquid ammonia, heat to 150°C and carry out high-pressure reaction; put the intermediate material into the concentration kettle, and carry out multiple distillations, the pressure of each distillation From high to low until methanol is successfully recovered, and the solution is centrifugally filtered; adding 70% sodium hydroxide to the centrifuged liquid to adjust the pH value to 14; performing rectification, extraction and dehydration under normal pressure And carry out secondary rectification again after purification, control secondary rectification as vacuum rectification to guarantee safety until collecting qualified cuts, obtain product product aminoacetaldehyde dimethyl acetal.

Embodiment 3

[0024] Add chloroacetaldehyde dimethyl acetal and methanol into the pressure reaction kettle, stir evenly; then add liquid ammonia, heat to 150°C and carry out high-pressure reaction; put the intermediate material into the concentration kettle, and carry out multiple distillations, the pressure of each distillation From high to low until methanol is successfully recovered, and the solution is centrifugally filtered; the concentration of 55% sodium hydroxide is added to the centrifuge to adjust the pH value to 13; rectification, extraction and dehydration are carried out under normal pressure And carry out secondary rectification again after purification, control secondary rectification as vacuum rectification to guarantee safety until collecting qualified cuts, obtain product product aminoacetaldehyde dimethyl acetal.

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Abstract

The invention discloses a preparation method of amino aminoacetaldehyde dimethyl acetal, comprising steps of firstly adding chloroacetaldehyde dimethyl acetal and methyl alcohol in a pressure reaction kettle, mixing them uniformly; then adding liquid ammonia, heating up to 150 degrees centigrade for high pressure reaction; adding intermediate materials into a concentration kettle, carrying out distillation several times, reducing the pressure of distillation each time until the methyl alcohol is recovered successfully, and centrifugally filtering the solution; adding sodium hydroxide in the centrifugal liquid to regulate its Ph value; conducting rectification and extraction dehydration under a normal pressure, and carrying out a secondary rectification after purification, maintaining the secondary rectification as a pressure reduced rectification to ensure safety until qualified distillate is collected, thereby obtaining the product amino aminoacetaldehyde dimethyl acetal. The preparation method is simple in process and is applicable to industrialization, with high product purity.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a preparation method of aminoacetaldehyde dimethyl acetal. Background technique [0002] Aminoacetaldehyde dimethyl acetal, also known as 2,2-dimethoxyethylamine and aminoacetaldehyde dimethyl acetal, has a molecular formula of C4H12NO2, and is the key to the synthesis of raw materials such as ifabradine hydrochloride and proprine analogues intermediate. The cost, safety performance, and simplicity brought by its preparation method have become the key links for it to participate in the preparation of other APIs as a key intermediate. Therefore, the improvement of its preparation method is of great significance. The existing method for producing aminoacetaldehyde dimethyl acetal mainly uses vinyl acetate as the starting material to generate the target product through bromination, synthesis and other processes, but the process is complicated, the cost is hig...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C213/10C07C217/40
CPCC07C213/02C07C213/10C07C217/40
Inventor 李一彪潘美玲
Owner FUJIAN WANKE PHARMA CO LTD
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