Preparation method of N,N-dibenzyl-ethylenediamin diacetate

A technology of dibenzylethylenediamine and dibenzylideneethylenediamine, which is applied in the N field, can solve the problems of low product yield, easy pollution of the environment, and high impurity content, and achieve high product yield, broad market prospects, The effect of low product impurity content

Inactive Publication Date: 2010-06-23
何永平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims at the disadvantages of low product yield, high impurity content in the product, easy pollution of the environment and the like in the method for preparing N,N-dibenzylethylenediaminediacetic acid in the prior art, and provides a method with simple operation and high product yield. High, low impurity content in the product, environmentally friendly preparation compound N, the method for N-dibenzylethylenediamine diacetic acid

Method used

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  • Preparation method of N,N-dibenzyl-ethylenediamin diacetate
  • Preparation method of N,N-dibenzyl-ethylenediamin diacetate

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Embodiment 1

[0023] Put 700kg of benzaldehyde and 200kg of ethylenediamine into a 2000L reactor, stir, react at a temperature of 120°C for 4 hours, cool, measure the solid weight to 786.0kg, put the resulting solid into a 5000L autoclave, add 2000kg of ethyl acetate, add 0.8kg catalyst Pd / c, hydrogenation reaction at a pressure of 0.5MPA and a temperature of 100°C for 4 hours, the solution was cooled, filtered, transferred to a 5000L reactor, added 400kg of glacial acetic acid, stirred and reacted at 80°C for 4 hours , cooled, stirred at 5° C. for 1 hour, filtered with suction, and dried to obtain 1105.6 kg of product with a yield of 93%.

Embodiment 2

[0025] Add 700g of benzaldehyde, 200g of ethylenediamine, and 1000g of ethyl acetate into a 3000ml three-necked flask, stir it magnetically, and react at a temperature of 80°C for 4 hours, then transfer the solution into a 5000ml autoclave, add 0.8g of catalyst Pd / c, and The pressure is 0.5MPA, the temperature is 100°C and hydrogenation reaction is carried out for 4 hours, the solution is cooled, filtered, transferred to a 5000ml three-necked flask, 1000g of ethyl acetate and 400g of glacial acetic acid are added, stirred and reacted at 80°C for 4 hours, cooled, Stir at 5° C. for 1 hour, and dry to obtain 1129.3 g of the product, with a yield of 95%.

Embodiment 3

[0027] Add 700g of benzaldehyde, 200g of ethylenediamine, and 1000g of ethyl acetate into a 3000ml three-necked flask, stir magnetically, react at a temperature of 80°C for 4 hours, then transfer the solution to a 5000ml autoclave, add 0.8g of catalyst Ni, 0.6MPA, hydrogenation reaction at 100°C for 4 hours, the solution was cooled, filtered, transferred to a 5000ml three-necked flask, added 1000g ethyl acetate, 400g glacial acetic acid, stirred and reacted at 80°C for 4 hours, cooled, at 5°C Stir for 1 hour, filter with suction, and dry to obtain 1099.6 g of the product, with a yield of 92.5%.

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Abstract

The invention relates to the field of chemical synthesis, in particular to a preparation method of N,N-dibenzyl-ethylenediamin diacetate. The preparation method comprises the following steps of: a: condensing reactants of benzaldehyde, ethylenediamine and glacial acetic acid into N,N-dibenzylidene ethylenediamine in an organic solvent; b: carrying out catalytic hydrogenation on the N,N-dibenzylidene ethylenediamine to obtain N,N-Dibenzylethylenediamine; and c: salifying the N,N-Dibenzylethylenediamine in the organic solvent to obtain the N,N-dibenzyl-ethylenediamin diacetate. The method has the advantages of simple and convenient operation, high product yield, low content of product impurity and no pollution to the environment, overcomes the defects existing in the prior art and has wide market prospect.

Description

technical field [0001] The invention relates to a preparation method of N, N-dibenzylethylenediamine diacetic acid. Background technique [0002] N,N-Dibenzylethylenediaminediacetic acid (abbreviated as DBED) is an important pharmaceutical intermediate, white needle crystal or powder, melting point 113-117°C, soluble in water and ethanol, slightly soluble in benzene, Acetone and ethyl acetate. Mainly used as pharmaceutical intermediates, used in the production of long-acting penicillin V, long-acting penicillin G, long-acting ampicillin and long-acting cephalosporins and other drugs, the existing synthesis of N,N-dibenzylethylenediaminediacetic acid The method is: use benzyl chloride, ethylenediamine and sodium hydroxide as raw materials to synthesize N,N-dibenzylethylenediamine, and then acidify in glacial acetic acid to obtain N,N-dibenzylethylenediaminediacetic acid. However, this method has the disadvantages of low product yield, high impurity content in the product, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/53C07C209/62C07C53/10
Inventor 何永平
Owner 何永平
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