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The synthetic method of n-ethylethylenediamine

A technology of ethylethylenediamine and a synthesis method, which is applied in the preparation of amino-substituted functional groups, organic chemistry, etc., can solve problems such as harsh reaction conditions, and achieve the effects of reducing the burden of post-processing, simple process, and good product selectivity.

Inactive Publication Date: 2011-11-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the acetic acid route method, an expensive catalyst must be used, and it must be operated in a high-pressure environment, and the reaction conditions are relatively harsh.

Method used

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  • The synthetic method of n-ethylethylenediamine
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  • The synthetic method of n-ethylethylenediamine

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Embodiment 1

[0025] The synthetic method of embodiment 1, N-ethylethylenediamine:

[0026] Add 110g (1.6mol) of ethylenediamine, 550g of methanol, and 60g (1.12mol) of sodium methoxide into a high-pressure reactor with a stirring temperature measuring device, and press 52g (0.8mol) of ethyl chloride after closing the lid; The internal temperature is raised to 40°C, and the pressure is 0.5Mpa at this time. Keep the temperature for 6 hours to complete the reaction, and the pressure after the reaction is 0.3Mpa.

[0027] After the reaction, the sodium chloride in the reaction liquid was filtered off, the filtrate was rectified, and the fraction at 128-130°C was collected to obtain 49.3 g of the product N-ethylethylenediamine with a yield of 69.89%.

[0028] The fraction collected at 62-64°C is methanol with a recovery rate of 84.26%; the fraction collected at 114-118°C is ethylenediamine with a recovery rate of 58.25%, both of which can be recycled.

Embodiment 2

[0029] The synthetic method of embodiment 2, N-ethylethylenediamine:

[0030] Add 110g (1.6mol) of ethylenediamine, 220g of methanol, and 47.5g (0.88mol) of sodium methylate into a high-pressure reactor with a stirring temperature measuring device. After closing the lid, press 52g (0.8mol) of ethyl chloride. The temperature was raised to 60°C within 1h, and the pressure was 0.7Mpa at this time. Keep the temperature for 3 hours to complete the reaction, and the pressure after the reaction is 0.36Mpa.

[0031] After the reaction, the sodium chloride in the reaction solution was filtered off, the filtrate was rectified, and the fraction at 128-130°C was collected to obtain 43.2 g of the product N-ethylethylenediamine with a yield of 61.25%.

[0032] At the same time, solvent methanol and excess ethylenediamine were collected, and the recoveries of the two were 84.54% and 58.12% respectively.

Embodiment 3

[0033] The synthetic method of embodiment 3, N-ethylethylenediamine:

[0034] Add 110g (1.6mol) of ethylenediamine, 550g of methanol, and 52g (0.96mol) of sodium methoxide into a high-pressure reaction kettle with a stirring temperature measuring device. After closing the lid of the kettle, press 52g (0.8mol) of ethyl chloride. The internal temperature was raised to 80°C, and the pressure was 1.2Mpa at this time. Keep the temperature for 4 hours to complete the reaction, and the pressure after the reaction is 0.5Mpa.

[0035] After the reaction, the sodium chloride in the reaction solution was filtered off, the filtrate was rectified, and the fraction at 128-130°C was collected to obtain 42.9 g of N-ethylethylenediamine, with a yield of 60.82%.

[0036] At the same time, solvent methanol and excess ethylenediamine were collected, and the recoveries of the two were 86.65% and 59.02% respectively.

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Abstract

The invention discloses a method for synthesizing 2-aminoethyl(ethyl)amine. The method comprises the following steps of: performing substitution reaction on raw materials of ethanediamine and chloroethane at the temperature of between 40 and 80DEG C under the pressure of between 0.2 and 2Mpa for 3 to 6 hours in a high pressure autoclave by taking alcohol as a solvent and sodium alcoholate as an acid binding agent, wherein a molar ratio of the ethanediamine to the chloroethane is (1.45-3.1):1, and a molar ratio of the chloroethane to the acid binding agent is 1:(1.09-1.4); and desalting and rectifying the obtained reaction product to obtain the 2-aminoethyl(ethyl)amine. The method for synthesizing the 2-aminoethyl(ethyl)amine has the characteristics of concise process, simple separation, high yield and the like.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing N-ethylethylenediamine. Background technique [0002] The molecular formula of N-ethylethylenediamine (referred to as NEED) is H 2 NCH 2 CH 2 NHCH 2 CH 3 , the structural formula is shown in S-1; colorless transparent liquid, specific gravity 0.837, refractive index 1.4385, boiling range (101.325KPa) 128-130°C, flash point 50°C, easily soluble in water. N-Ethylethylenediamine (NEED) is an important intermediate in the synthesis of many antibiotics, one of the basic raw materials for cefoperazone of cephalosporins, piperacillin of penicillins and cefbuperazone of cephamycin derivatives That is N-ethylethylenediamine. [0003] [0004] Comprehensive literature report, the preparation of N-ethylethylenediamine mainly adopts following method at present: [0005] (1) Taking ethylamine and aminoethylsulfuric acid as raw materials, water ...

Claims

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Application Information

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IPC IPC(8): C07C211/10C07C209/08
Inventor 陈新志徐庐峰黄佳民钱超
Owner ZHEJIANG UNIV
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