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Preparation method of N,N-dibenzyl ethylenediamine diacetate

A technology of dibenzylethylenediamine and acetate is applied in the preparation of carboxylate, carboxylate, amino compound, etc., can solve problems such as high cost, harsh conditions, etc., improve yield, reduce reaction Cost, effect of improving safety

Active Publication Date: 2018-09-21
SICHUAN WUSHENG CHUNRUI MEDICAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to use an autoclave for hydrogenation, the conditions are harsh, and it is heated for a long time, so the cost is high

Method used

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

Examples

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Effect test

Embodiment

[0030] A kind of preparation method of N,N-dibenzylethylenediamine diacetate, its method step is as follows:

[0031]

[0032] S1. Add 50 parts by weight of diacetyldibenzylethylenediamine material into the three-necked bottle, add 80-120 parts by weight of concentrated hydrochloric acid with a concentration of 30% to 31% into the three-necked bottle, and then slowly heat up the three-necked bottle to 72 ~76°C, react for 5 hours after heating up, then cool the three-neck flask to 0~3°C with cooling water, and then filter to obtain 36.0~37.5 parts by weight of compound B;

[0033] S2. Add 36.0 to 37.5 parts by weight of compound B obtained in step S1 into 200 parts by weight of water to fully dissolve, and add dropwise a sodium hydroxide solution 5.2 to 5.6 with a concentration of 97.5% to 98.5% at a temperature of 10 to 20°C. parts by weight, adjust the pH value to 8-9; after the pH value is adjusted, add 50 parts by weight of toluene for the first extraction and layering t...

Embodiment 1

[0036] A kind of preparation method of N,N-dibenzylethylenediamine diacetate, its method step is as follows:

[0037] S1. Add 50g of diacetyldibenzylethylenediamine material into a 1000ml three-necked bottle, add 100g of concentrated hydrochloric acid with a concentration of 30% to 31% into the three-necked bottle, then slowly heat up the three-necked bottle to 74°C, and react after heating After 5 hours, the temperature of the three-neck flask was lowered to 3°C with cooling water, and then filtered to obtain 37.3 g of compound B;

[0038] S2. Add 37.3 g of compound B obtained in step S1 to 200 g of water to fully dissolve, add dropwise 5.4 g of sodium hydroxide solution with a concentration of 97.5% to 98.5% at a temperature of 15°C, and adjust the pH value to 8.5; After the pH value has been adjusted, add 50g of toluene for the first extraction and layering treatment; after the first extraction and layering treatment are completed, then add 50g of toluene for the second ext...

Embodiment 2

[0043] A kind of preparation method of N,N-dibenzylethylenediamine diacetate, its method step is as follows:

[0044] S1. Add 50g of diacetyldibenzylethylenediamine material into the three-necked flask, add 120g of concentrated hydrochloric acid with a concentration of 30% to 31% into the there-necked flask, then slowly raise the temperature to 76°C in the there-necked flask, and react for 5 hour, then cooled the three-necked flask to 1.5°C with cooling water, and then filtered to obtain 37.3g of compound B;

[0045] S2. Add 37.3 g of compound B obtained in step S1 to 200 g of water to fully dissolve, add dropwise 5.4 g of sodium hydroxide solution with a concentration of 97.5% to 98.5% at a temperature of 20° C., and adjust the pH value to 9; After the pH value has been adjusted, add 50g of toluene for the first extraction and layering treatment; after the first extraction and layering treatment are completed, then add 50g of toluene for the second extraction and layering tre...

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Abstract

The invention discloses a preparation method of N,N-dibenzyl ethylenediamine diacetate. The method comprises the following steps: S1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine material into a three-necked bottle, and adding 80-120 parts by weight of concentrated hydrochloric acid into the three-necked bottle to obtain 36.0-37.5 parts by weight of a compound B; S2, adding 200 parts by weight of water into the compound B obtained in the step S1 for fully dissolving, and dropwise adding a sodium hydroxide solution to adjust the pH value to 8-9; then, adding toluene for extracting for a plurality of times, and carrying out layered treatment to obtain an organic phase of a mixture of a compound C and the toluene; S3, adding the organic phase of the mixture of the compound Cand toluene into the three-necked bottle and distilling under the reduced pressure until no fraction is obtained, then adding ethyl acetate for dissolving, heating up to 60 DEG C, then dropwise adding 20 parts by weight of glacial acetic acid, and drying to obtain 47.0-49.0 parts by weight of dibenzyl ethylenediamine diacetate finally. The preparation method provided by the invention improves thereaction safety and reduces the reaction cost; furthermore, the yield of the dibenzyl ethylenediamine diacetate is also increased to 93% or above.

Description

technical field [0001] The invention relates to a method for synthesizing medicine, in particular to a method for preparing N,N-dibenzylethylenediamine diacetate. Background technique [0002] N,N-dibenzylethylenediamine diacetate (DBED for short) is mainly used as a pharmaceutical intermediate for the production of long-acting penicillin G, long-acting penicillin V, long-acting ampicillin, long-acting cephalosporins and other drugs . "Study on the Synthesis of N,N-Dibenzylethylenediamine Diacetate" by Wang Renming et al., Jiangxi Chemical Industry, 2002 (2) records that N, N-dibenzylethylenediamine, and then salted with acetic acid to obtain N, N-dibenzylethylenediamine diacetate. The yield of this method is low, and there are relatively high by-products of monobenzylethylenediamine, tribenzylethylenediamine and tetrabenzylethylenediamine. Chinese patent 201010300046.7 records that N,N-dibenzylideneethylenediamine is synthesized from benzaldehyde and ethylenediamine as r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/27C07C209/68C07C209/62C07C53/10C07C51/41
CPCC07C51/412C07C209/62C07C209/68C07C211/27C07C53/10
Inventor 朱泽文胡奎赵勇郭小刚黄瑜周刘阳
Owner SICHUAN WUSHENG CHUNRUI MEDICAL CHEM
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