Method for preparing 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, and difficulty in industrialization, and achieve low cost, simple process route, and cheap raw materials and auxiliary materials Easy to get effect

Inactive Publication Date: 2014-04-23
JIANGSU CHENGXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process uses the highly toxic bromine and the process is complicated, the cost is high, and it is not easy to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 400g of 10% aqueous ammonia solution into a 500ml autoclave, and then add 20g of chloroacetaldehyde dimethyl acetal at one time. Under stirring, the temperature of the reaction solution is raised to 135-140°C, and the temperature is controlled and stirred for 5 hours. Distill the reaction solution until no obvious fractions are distilled out, recover 220g of ammonia water, weigh 20g of 30% liquid caustic soda aqueous solution and add it to the remaining reaction solution, adjust the pH of the reaction solution to 14, rectify at atmospheric pressure, and collect a colorless transparent liquid 8.6g. The yield of aminoacetaldehyde dimethyl acetal in this embodiment is 47.4%.

Embodiment 2

[0019] Add 350g of 30% aqueous ammonia solution into a 500ml autoclave, and then add 30g of chloroacetaldehyde dimethyl acetal at one time. With stirring, the temperature of the reaction solution is raised to 145-150°C, and the temperature is controlled and stirred for 5 hours. Distill the reaction solution until no obvious fractions are distilled out, recover 190g of ammonia water, weigh 30g of 40% liquid caustic soda solution and add it to the remaining reaction solution, adjust the pH of the reaction solution to 14, rectify at atmospheric pressure, and collect a colorless transparent liquid 15g. The yield of aminoacetaldehyde dimethyl acetal in this example is 59.2%.

Embodiment 3

[0021] Add 350g of 40% aqueous ammonia solution into a 500ml autoclave, and then add 40g of chloroacetaldehyde dimethyl acetal at one time. With stirring, the temperature of the reaction solution is raised to 130-135°C, and the temperature is controlled and stirred for 3 hours. Distill the reaction solution until no obvious fractions are distilled out, recover 175g of ammonia water, weigh 40g of 50% liquid caustic soda aqueous solution and add it to the remaining reaction solution, adjust the pH of the reaction solution to 14, rectify at atmospheric pressure, and collect a colorless transparent liquid 24g. The yield of aminoacetaldehyde dimethyl acetal in this example is 71.1%.

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PUM

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Abstract

The invention relates to a method for preparing aminoacetaldehyde dimethyl acetal, which comprises the following steps: 1) adding dimethyl chloroacetal and an ammonia aqueous solution with a concentration of 10-40% into a container at a time, uniformly stirring; 2) stirring the reaction solution in step 1), heating the reaction solution to 100-150 DEG C; 3) performing distillation of the reaction solution in step 2), recovering the ammonia water till no obvious fraction is distilled out; 4) adding a sodium hydroxide aqueous solution with a concentration of 20%-50% into the reaction solution in step 3), adjusting the pH to 12-14; 5) performing rectification of the solution in step 4), and collecting colorless and light yellow transparent liquid which is the target product of aminoacetaldehyde dimethyl acetal.

Description

technical field [0001] The technology of the invention relates to the technical field of medicine and chemical industry. Background technique [0002] Aminoacetaldehyde dimethyl acetal (also known as: 2,2-dimethoxyethylamine), the molecular formula is: C 4 h 11 NO 2 It is a key intermediate for the synthesis of ivabradine hydrochloride, proline analogs and praziquantel and other raw materials. Therefore, it is of certain significance to synthesize aminoacetaldehyde dimethyl acetal with a low-cost, simple and safe production process. However, the existing process for producing aminoacetaldehyde dimethyl acetal uses vinyl acetate as a starting material, and synthesizes the target product through bromination, Gabriel synthesis, and hydrazinolysis. This process uses bromine, a highly toxic substance, and the process is complex and costly, and it is not easy to realize industrialization. Contents of the invention [0003] Purpose of the invention: In order to overcome the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/40C07C213/02
Inventor 许刘华刘明明邢将军刘加根
Owner JIANGSU CHENGXIN PHARMA
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