CN108558676B - Preparation method of N, N-dibenzylethylenediamine diacetate - Google Patents
Preparation method of N, N-dibenzylethylenediamine diacetate Download PDFInfo
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Abstract
The invention discloses a preparation method of N, N-dibenzyl ethylenediamine diacetate, 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 compound B; s2, adding 200 parts by weight of water into the compound B obtained in the step S1 for full dissolution, and dropwise adding a sodium hydroxide solution to adjust the pH value to 8-9; adding toluene, extracting for many times, and carrying out layering treatment to obtain a compound C and toluene mixture organic phase; and S3, adding the organic phase of the mixture of the compound C and toluene into a three-neck flask, distilling under reduced pressure until no fraction is produced, adding ethyl acetate to dissolve the organic phase, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and drying to obtain 47.0-49.0 parts by weight of dibenzylethylenediamine diacetate. The invention improves the safety of the reaction, reduces the reaction cost, and improves the yield of the dibenzyl ethylenediamine diacetate to more than 93 percent.
Description
Technical Field
The invention relates to a synthesis method of a medicament, in particular to a preparation method of N, N-dibenzylethylenediamine diacetate.
Background
N, N-dibenzylethylenediamine diacetate (DBED) is mainly used as a medical intermediate and is applied to producing long-acting penicillin G, long-acting penicillin V, long-acting ampicillin, long-acting cephalo-type medicaments and other medicaments. Wangxing et al, research on the synthesis of N, N-dibenzylethylenediamine diacetate (2002 (2)) described that benzyl chloride, ethylenediamine and sodium hydroxide were used as raw materials to synthesize N, N-dibenzylethylenediamine, which was then salified with acetic acid to obtain N, N-dibenzylethylenediamine diacetate. The method has lower yield and higher by-products of the monobenzyl ethylenediamine, the tribenzyl ethylenediamine and the tetrabenzyl ethylenediamine. Chinese patent 201010300046.7 describes that N, N-dibenzylidene ethylenediamine is synthesized from benzaldehyde and ethylenediamine, and then hydrogenated under the catalysis of a catalyst to obtain N, N-dibenzylidene ethylenediamine, which is then salified with acetic acid to obtain N, N-dibenzylidene ethylenediamine diacetate. The method uses an autoclave for hydrogenation, and has the disadvantages of harsh conditions, long-time heating and high cost. This study improved the process for the reduction of N, N '-dibenzylidene ethylenediamine to N, N' -dibenzylidene ethylenediamine based on the second route.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the preparation method of the N, N-dibenzyl ethylenediamine diacetate, the invention obtains the primary dibenzyl ethylenediamine diacetate by taking diacetyl dibenzyl ethylenediamine as a raw material, regulating the pH value, extracting toluene twice, dissolving ethyl acetate, adding glacial acetic acid for reaction, and then drying to obtain the dibenzyl ethylenediamine diacetate, thereby improving the reaction safety, reducing the reaction cost and improving the yield of the dibenzyl ethylenediamine diacetate to more than 93 percent.
The purpose of the invention is realized by the following technical scheme:
a preparation method of N, N-dibenzyl ethylenediamine diacetate comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 80-120 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 72-76 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 0-3 ℃ by using cooling water, and filtering to obtain 36.0-37.5 parts by weight of a compound B;
s2, adding 200 parts by weight of water to fully dissolve 36.0-37.5 parts by weight of the compound B obtained in the step S1, dropwise adding 5.2-5.6 parts by weight of a 97.5-98.5% sodium hydroxide solution at 10-20 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 0.9-1.1 hour under heat preservation after dropwise adding; and then slowly cooling to 5 ℃, filtering to obtain 49.3-49.7 parts by weight of wet dibenzyl ethylenediamine diacetate, and drying at the temperature of 40-45 ℃ to finally obtain 47.0-49.0 parts by weight of dibenzyl ethylenediamine diacetate.
The first preferable preparation method of the N, N-dibenzyl ethylenediamine diacetate comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 100 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 74 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 3 ℃ by using cooling water, and filtering to obtain 37.3 parts by weight of a compound B;
s2, adding 200 parts by weight of water to sufficiently dissolve 37.3 parts by weight of the compound B obtained in the step S1, dropwise adding 5.4 parts by weight of a 97.5-98.5% sodium hydroxide solution at 15 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 0.9 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.5 weight parts of wet dibenzyl ethylenediamine diacetate, and drying at the temperature of 43 ℃ to finally obtain 48.0 weight parts of dibenzyl ethylenediamine diacetate.
The second preferred preparation method of N, N-dibenzylethylenediamine diacetate comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine material into a three-necked bottle, adding 120 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 76 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 1.5 ℃ by using cooling water, and filtering to obtain 37.3 parts by weight of a compound B;
s2, adding 200 parts by weight of water to sufficiently dissolve 37.3 parts by weight of the compound B obtained in the step S1, dropwise adding 5.4 parts by weight of a 97.5-98.5% sodium hydroxide solution at the temperature of 20 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-necked bottle, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 1.0 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.5 weight parts of wet dibenzyl ethylenediamine diacetate, and drying at 45 ℃ to finally obtain 49.0 weight parts of dibenzyl ethylenediamine diacetate.
The third method for preparing the N, N-dibenzyl ethylenediamine diacetate is preferably implemented by the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 80 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 72 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 0.5 ℃ by using cooling water, and filtering to obtain 36 parts by weight of compound B;
s2, adding 200 parts by weight of water to fully dissolve 36 parts by weight of the compound B obtained in the step S1, dropwise adding 5.4 parts by weight of a 97.5-98.5% sodium hydroxide solution at 10 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 1.1 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.5 weight parts of wet dibenzyl ethylenediamine diacetate, and drying at the temperature of 40 ℃ to finally obtain 47.0 weight parts of dibenzyl ethylenediamine diacetate.
Preferably, the concentration of glacial acetic acid in the step S3 is 98%.
The weight portion of the invention is gram or kilogram.
The reagents of the invention are all conventional reagents which are commercially available.
The percentage concentrations (solution concentrations) described in the present invention are all weight percentage concentrations.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, diacetyl dibenzyl ethylenediamine is used as a raw material, hydrochloric acid is used, the pH value is adjusted, toluene is extracted twice, ethyl acetate is dissolved, glacial acetic acid is added for reaction to obtain a primary dibenzyl ethylenediamine diacetate product, and the primary dibenzyl ethylenediamine diacetate product is dried to obtain the dibenzyl ethylenediamine diacetate, so that the reaction safety is improved, the reaction cost is reduced, and the yield of the dibenzyl ethylenediamine diacetate is improved to more than 93%.
Detailed Description
The present invention will be described in further detail with reference to examples.
Examples
A preparation method of N, N-dibenzyl ethylenediamine diacetate comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 80-120 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 72-76 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 0-3 ℃ by using cooling water, and filtering to obtain 36.0-37.5 parts by weight of a compound B;
s2, adding 200 parts by weight of water to fully dissolve 36.0-37.5 parts by weight of the compound B obtained in the step S1, dropwise adding 5.2-5.6 parts by weight of a 97.5-98.5% sodium hydroxide solution at 10-20 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 0.9-1.1 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.3-49.7 weight parts of wet dibenzyl ethylenediamine diacetate (namely, the compound D containing moisture), and drying at the temperature of 40-45 ℃ to finally obtain 47.0-49.0 weight parts of dibenzyl ethylenediamine diacetate (namely, the compound D). The dibenzyl ethylenediamine diacetate obtained by the invention is white crystalline powder or white needle-shaped crystals, and the quality standard of the dibenzyl ethylenediamine diacetate is met through inspection, and the yield of the dibenzyl ethylenediamine diacetate reaches more than 93%.
Example one
A preparation method of N, N-dibenzyl ethylenediamine diacetate comprises the following steps:
s1, adding 50g of diacetyl dibenzyl ethylenediamine into a 1000ml three-necked bottle, adding 100g of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 74 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 3 ℃ by using cooling water, and filtering to obtain 37.3g of compound B;
s2, adding 200g of water into 37.3g of the compound B obtained in the step S1 for full dissolution, dropwise adding 5.4g of a 97.5-98.5% sodium hydroxide solution at the temperature of 15 ℃, and adjusting the pH value to 8.5; after the pH value is adjusted, adding 50g of toluene for carrying out first extraction and layering treatment; after the first extraction and the layering treatment are finished, adding 50g of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase, wherein the compound C and the compound B are the same chemical substance;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-necked bottle, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200g of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20g of glacial acetic acid, wherein the concentration of the glacial acetic acid is 98%, and carrying out heat preservation reaction for 0.9 hour after the dropwise adding is finished; then slowly cooling to 5 deg.C, filtering to obtain 49.5g wet product of dibenzyl ethylenediamine diacetate (i.e. compound D containing moisture), and drying at 43 deg.C to obtain 48.0g wet product of dibenzyl ethylenediamine diacetate (i.e. compound D). The dibenzyl ethylenediamine diacetate obtained in this example was a white crystalline powder or white needle-like crystals, and the following compositional tests were performed on the dibenzyl ethylenediamine diacetate obtained in this example, as shown in the following table:
the quality standard of the dibenzyl ethylenediamine diacetate is met through inspection, and the yield of the dibenzyl ethylenediamine diacetate reaches 95 percent and the content of the dibenzyl ethylenediamine diacetate is 99.78 percent.
Example two
A preparation method of N, N-dibenzyl ethylenediamine diacetate comprises the following steps:
s1, adding 50g of diacetyl dibenzyl ethylenediamine material into a three-necked bottle, adding 120g of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 76 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 1.5 ℃ by using cooling water, and filtering to obtain 37.3g of compound B;
s2, adding 200g of water into 37.3g of the compound B obtained in the step S1 for full dissolution, dropwise adding 5.4g of a 97.5-98.5% sodium hydroxide solution at the temperature of 20 ℃, and adjusting the pH value to 9; after the pH value is adjusted, adding 50g of toluene for carrying out first extraction and layering treatment; after the first extraction and layering treatment, adding 50g of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-necked bottle, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200g of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20g of glacial acetic acid, wherein the concentration of the glacial acetic acid is 98%, and carrying out heat preservation reaction for 1.0 hour after the dropwise adding is finished; then slowly cooling to 5 deg.C, filtering to obtain 49.5g wet product of dibenzyl ethylenediamine diacetate (i.e. compound D containing moisture), and drying at 45 deg.C to obtain 49.0g wet product of dibenzyl ethylenediamine diacetate (i.e. compound D).
The dibenzyl ethylenediamine diacetate obtained in this example was a white crystalline powder or white needle-like crystals, and the following compositional tests were performed on the dibenzyl ethylenediamine diacetate obtained in this example, as shown in the following table:
the test proves that the product meets the quality standard of dibenzyl ethylenediamine diacetate, and the yield of the dibenzyl ethylenediamine diacetate reaches 96.91 percent, and the content of the dibenzyl ethylenediamine diacetate is 99.94 percent.
EXAMPLE III
A preparation method of N, N-dibenzyl ethylenediamine diacetate comprises the following steps:
s1, adding 50g of diacetyl dibenzyl ethylenediamine material into a three-necked bottle, adding 80g of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 72 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 0.5 ℃ by using cooling water, and filtering to obtain 36g of compound B;
s2, adding 200g of water into 36g of the compound B obtained in the step S1 for full dissolution, dropwise adding 5.4g of a 97.5-98.5% sodium hydroxide solution at the temperature of 10 ℃, and adjusting the pH value to 8; after the pH value is adjusted, adding 50g of toluene for carrying out first extraction and layering treatment; after the first extraction and layering treatment, adding 50g of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-necked bottle, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200g of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20g of glacial acetic acid, wherein the concentration of the glacial acetic acid is 98%, and carrying out heat preservation reaction for 1.1 hours after the dropwise adding is finished; then slowly cooling to 5 deg.C, filtering to obtain 49.5g wet product of dibenzyl ethylenediamine diacetate (i.e. compound D containing moisture), and drying at 40 deg.C to obtain 47.0g wet product of dibenzyl ethylenediamine diacetate (i.e. compound D).
The dibenzyl ethylenediamine diacetate obtained in this example was a white crystalline powder or white needle-like crystals, and the following compositional tests were performed on the dibenzyl ethylenediamine diacetate obtained in this example, as shown in the following table:
the quality standard of the dibenzyl ethylenediamine diacetate is met through inspection, and the yield of the dibenzyl ethylenediamine diacetate reaches 93 percent and the content is 99.84 percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. A preparation method of N, N-dibenzyl ethylenediamine diacetate is characterized by comprising the following steps: the method comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 80-120 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 72-76 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 0-3 ℃ by using cooling water, and filtering to obtain 36.0-37.5 parts by weight of a compound B;
s2, adding 200 parts by weight of water to fully dissolve 36.0-37.5 parts by weight of the compound B obtained in the step S1, dropwise adding 5.2-5.6 parts by weight of a 97.5-98.5% sodium hydroxide solution at 10-20 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, wherein the concentration of the glacial acetic acid is 98%, and carrying out heat preservation reaction for 0.9-1.1 hours after the glacial acetic acid is dropwise added; and then slowly cooling to 5 ℃, filtering to obtain 49.3-49.7 parts by weight of wet dibenzyl ethylenediamine diacetate, and drying at the temperature of 40-45 ℃ to finally obtain 47.0-49.0 parts by weight of dibenzyl ethylenediamine diacetate.
2. The process for producing N, N-dibenzylethylenediamine diacetate according to claim 1, wherein: the method comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 100 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 74 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 3 ℃ by using cooling water, and filtering to obtain 37.3 parts by weight of a compound B;
s2, adding 200 parts by weight of water to sufficiently dissolve 37.3 parts by weight of the compound B obtained in the step S1, dropwise adding 5.4 parts by weight of a 97.5-98.5% sodium hydroxide solution at 15 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 0.9 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.5 weight parts of wet dibenzyl ethylenediamine diacetate, and drying at the temperature of 43 ℃ to finally obtain 48.0 weight parts of dibenzyl ethylenediamine diacetate.
3. The process for producing N, N-dibenzylethylenediamine diacetate according to claim 1, wherein: the method comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine material into a three-necked bottle, adding 120 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 76 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 1.5 ℃ by using cooling water, and filtering to obtain 37.3 parts by weight of a compound B;
s2, adding 200 parts by weight of water to sufficiently dissolve 37.3 parts by weight of the compound B obtained in the step S1, dropwise adding 5.4 parts by weight of a 97.5-98.5% sodium hydroxide solution at the temperature of 20 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-necked bottle, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 1.0 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.5 weight parts of wet dibenzyl ethylenediamine diacetate, and drying at 45 ℃ to finally obtain 49.0 weight parts of dibenzyl ethylenediamine diacetate.
4. The process for producing N, N-dibenzylethylenediamine diacetate according to claim 1, wherein: the method comprises the following steps:
s1, adding 50 parts by weight of diacetyl dibenzyl ethylenediamine into a three-necked bottle, adding 80 parts by weight of concentrated hydrochloric acid with the concentration of 30% -31% into the three-necked bottle, slowly heating the three-necked bottle to 72 ℃, reacting for 5 hours after heating, cooling the three-necked bottle to 0.5 ℃ by using cooling water, and filtering to obtain 36 parts by weight of compound B;
s2, adding 200 parts by weight of water to fully dissolve 36 parts by weight of the compound B obtained in the step S1, dropwise adding 5.4 parts by weight of a 97.5-98.5% sodium hydroxide solution at 10 ℃, and adjusting the pH value to 8-9; after the pH value is adjusted, adding 50 parts by weight of toluene to perform first extraction and layering treatment; after the first extraction and layering treatment, adding 50 parts by weight of toluene for second extraction and layering treatment to obtain a compound C and toluene mixture organic phase;
s3, adding the organic phase of the mixture of the compound C and toluene obtained in the step S2 into a three-neck flask, distilling under reduced pressure until no fraction is obtained, cooling to 30 ℃, adding 200 parts by weight of ethyl acetate to dissolve, heating to 60 ℃, dropwise adding 20 parts by weight of glacial acetic acid, and reacting for 1.1 hour under heat preservation after dropwise adding; then slowly cooling to 5 ℃, filtering to obtain 49.5 weight parts of wet dibenzyl ethylenediamine diacetate, and drying at the temperature of 40 ℃ to finally obtain 47.0 weight parts of dibenzyl ethylenediamine diacetate.
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