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Preparation method of N,N-diethylethylenediamine

A technology of diethylethylenediamine and diethylamine, applied in the field of organic compound preparation, can solve the problems of high price of bromoethylamine bromate, unsuitable for industrial production, difficult to handle, etc., and achieves high yield and low cost of raw materials , the effect of simple operation

Inactive Publication Date: 2014-11-26
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has a high yield, but the bromoethylammonium bromate used is expensive, and the reaction generates copper sulfide, which is not easy to handle and is not suitable for industrial production

Method used

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  • Preparation method of N,N-diethylethylenediamine
  • Preparation method of N,N-diethylethylenediamine

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Embodiment 1

[0024] Embodiment 1, the preparation method of N, N-diethylethylenediamine

[0025] Add 0.60 mol of diethylamine, 0.15 mol of 2-chloroethylamine hydrochloride, sodium methoxide methanol solution (containing 0.15 mol of sodium methoxide and 40 mL of methanol), and 0.3 g (0.003 mol) of cuprous chloride into the autoclave. Then close the lid of the kettle, start stirring after leak detection, heat to 150°C, and increase the pressure to about 1.0MPa. The reaction was continued for 5 hours, and the reaction pressure did not change substantially during the process. After the reaction, stop heating, after cooling to room temperature, stop stirring, open the kettle, pour out the reaction solution, add saturated sodium hydroxide solution until the pH is ≥ 13 (that is, it is strongly alkaline), the purpose is to neutralize the product Hydrochloric acid, natural layering, the upper oil layer and the lower water layer are obtained; the target product is located in the oil layer, the oil ...

Embodiment 2~ Embodiment 12

[0027] Change the consumption of the diethylamine in embodiment 1, 2-chloroethylamine hydrochloride and sodium methylate methanol solution, change the kind of catalyzer and consumption or cancel use catalyzer, also changed temperature of reaction, reaction pressure and reaction time, thereby Get the corresponding example. The specific data and the final yield are shown in Table 1.

[0028] Table 1

[0029]

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Abstract

The invention discloses a preparation method of N,N-diethylethylenediamine, which comprises the following steps: carrying out reaction on raw materials diethylamine and 2-chlorethamin hydrochloride in a high-pressure autoclave by using a sodium methoxide methanol solution as an acid binding agent at 100-200 DEG C under the reaction pressure of 0.52-1.60 MPa for 3-8 hours, wherein the mol ratio of diethylamine to 2-chlorethamin hydrochloride is (1-8):1, and the mol ratio of sodium methoxide in the sodium methoxide methanol solution to 2-chlorethamin hydrochloride is (0.9-1.1):1; and regulating the pH value of the reaction solution to at least 13 with alkali liquor, stratifying to obtain an oil phase, and rectifying the oil phase to obtain the N,N-diethylethylenediamine. The method disclosed by the invention has the characteristics of low raw material cost, high yield, high economy and safety and the like, and is simple to operate and easy to implement.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, and in particular relates to a preparation method of N,N-diethylethylenediamine. Background technique [0002] N,N-Diethylethylenediamine is an important fine chemical intermediate, which is used in the fields of medicine, surfactants and coatings. Metoclopramide and Tiapride can be used in the textile industry to synthesize chromebimin BCH and cationic surfactants, and can be used as curing agents and chelating agents for epoxy powder coatings in coatings. The preparation of this compound mainly contains following several methods at present: [0003] a. Cyanomethylation and reduction of diethylamine: This method was published by Bloom M S in 1945. The synthesis process is divided into two steps: 1) Synthesis of dialkylamino acetonitrile: formaldehyde and sodium bisulfite synthesis Sodium hydroxymethanesulfonate, dialkylamine replaces hydroxyl to obtain dialkylaminomethanesulfonate, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/10C07C209/08
Inventor 钱超王亚运陈新志
Owner ZHEJIANG UNIV
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