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Green preparing method for high-purity N,N'-dibenzyl ethylenediamine diacetate

A technology of dibenzylethylenediamine hydrochloride and dibenzylethylenediamine is applied in the field of green preparation of high-purity N,N'-dibenzylethylenediaminediacetic acid, and can solve the harm to operators and the environment , by-products are difficult to handle, difficult to produce and store, etc., to achieve the effect of low production cost, reduction of by-products or waste, and easy operation

Active Publication Date: 2018-11-06
重庆天地药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above-mentioned three methods all can make DBED, but it has different shortcoming: the raw material of method one is easy to get, but will carry out hydrogenation reaction with precious metal catalyst, this operation is not easy to control, and production cost is high; Method two will use 1, 2-dibromoethane, though the yield is high, the raw material is not easy to get, and the by-product is more difficult to handle; the method benzyl trichloride is an active substance, which is not only difficult to produce and store, the raw material is not easy to get, and it is very easy to cause allergies during production simultaneously, which will Cause greater harm to operators and the environment

Method used

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  • Green preparing method for high-purity N,N'-dibenzyl ethylenediamine diacetate

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Embodiment 1

[0027] 1. Preparation of free base N,N'-dibenzylethylenediamine:

[0028] Add 420ml of drinking water to a 1000ml reaction bottle, put in 60g of N,N'-dibenzylethylenediamine hydrochloride, control the temperature of the material not to exceed 40°C; then control the temperature at 25°C and add 90g of ammonia water dropwise, and the dropwise addition is completed , continue to stir for 30 minutes; add 540g of dichloromethane, stir for 30 minutes, and let stand for 15 minutes. After the materials are separated, the lower organic layer is transferred to a 1000ml concentration bottle, and the temperature is controlled at 60°C. , to N, N'-dibenzylethylenediamine solution.

[0029] 2. Preparation of N,N'-dibenzylethylenediaminediacetic acid:

[0030] Put 420g of methyl acetate into the concentrated bottle, control the temperature at 30°C and dissolve it. After the dissolution time is 30 minutes, add 28g of acetic acid dropwise at 30°C to form a salt reaction. The dropwise addition t...

Embodiment 2

[0032] 1. Preparation of free base N,N'-dibenzylethylenediamine:

[0033] Add 420L of drinking water to the 1000L reaction kettle, put in 60kg of N,N'-dibenzylethylenediamine sulfate, control the temperature of the material not to exceed 40°C; then control the temperature at 40°C and add 90kg of sodium hydroxide dropwise, and the dropwise addition is completed , continue to stir for 60 minutes; add 540 kg of chloroform, stir for 60 minutes, and let stand for 20 minutes. After the materials are separated, the lower organic layer is transferred to a 1000L concentration kettle, and the temperature is controlled at 40 ° C. Steam 480 kg of organic phase chloroform , to N, N'-dibenzylethylenediamine solution.

[0034] 2. Preparation of N,N'-dibenzylethylenediaminediacetic acid:

[0035] Put 420kg of methyl acetate into the concentrated reaction tank, control the temperature at 60°C to dissolve, and after the dissolution time is 90 minutes, add 28kg of acetic acid dropwise at 0°C to...

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Abstract

The invention relates to a green preparing method for high-purity N,N'-dibenzyl ethylenediamine diacetate. A by-product N,N'-dibenzyl ethylenediamine dihydrochloride or N,N'-dibenzyl ethylenediamine sulfate generated in the production process of long-acting cephalosporin medicine is used, and is neutralized, extracted and concentrated, then the product and acetic acid are mixed to form salt, and the high-purity N,N'-dibenzyl ethylenediamine diacetate is prepared. According to the green preparing method, discharging of liquid and solid waste is reduced, regeneration of the N,N'-dibenzyl ethylenediamine diacetate and recycling of waste are achieved, generation of the by-product or waste is reduced from the source, and therefore the aim of protecting and improving the environment is achieved.Compared with a traditional preparing method, the green preparing method has the advantages that the raw material is easy to obtain, the technology is simple, operation is easy and convenient, the production cost is low, and the green preparing method is more suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of an intermediate in the fields of medicine and chemical industry, in particular to a green preparation method of high-purity N,N'-dibenzylethylenediaminediacetic acid. Background technique [0002] N,N'-dibenzylethylenediaminediacetic acid (DBED for short) is an important chemical reagent, chemical intermediate, material intermediate, and an important intermediate for products such as benzathine penicillin. There are mainly three synthetic routes about the synthetic method of DBED: [0003] Method 1: DBED is obtained from the condensation of benzaldehyde and ethylenediamine through hydrogenation reduction, and then salified with acetic acid to obtain the target product. The reaction formula is as follows: [0004] [0005] Method two, benzylamine is condensed with 1,2-dibromoethane, and then salified with acetic acid to obtain the target product DBED, the reaction formula is as follows: [0006] [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/09C07C51/41C07C53/10
CPCC07C51/412C07C209/00C07C211/09C07C53/10
Inventor 岑勇白智全刘悉承卢福生刘鑫石航胡建黎鹏辉周伦海王军
Owner 重庆天地药业有限责任公司
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