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Preparation method of 2-(aminoxy) ethanol

A technology of amino-oxygen and ethanol, which is applied in the direction of organic chemistry, can solve the problems of low product purity and low reaction yield, and achieve the effects of simple operation, low cost and less pollution

Inactive Publication Date: 2014-01-29
纪兴国
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Problems solved by technology

The synthesis method of 2-(aminooxy)ethanol in the prior art has the defects of low reaction yield and low product purity

Method used

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  • Preparation method of 2-(aminoxy) ethanol

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Embodiment Construction

[0018] The present invention will be described in detail below with reference to specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but do not limit the present invention in any form. It should be noted that, for those skilled in the art, several modifications and improvements can be made without departing from the concept of the present invention. These all belong to the protection scope of the present invention.

[0019] A kind of preparation method of 2-(amino oxygen) ethanol, comprises the following steps (as figure 1 shown):

[0020] Step (1), sequentially add 1 weight part of N-hydroxyphthalamide, 4 weight parts of DMF (dimethylformamide) and 1.24 weight parts of TEA (triethylamine) to the reactor;

[0021] Step (2), heating the reaction kettle to 60°C, adding 1.152 parts by weight of 2-bromoethanol dropwise, controlling the reaction temperature to <95°C;

[0022] Step (3), after the dropwise a...

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Abstract

The invention relates to a preparation method of 2-(aminoxy) ethanol. The preparation method comprises the following steps: sequentially adding N-hydroxyphthalimide, dimethyl formamide (DMF) and triethylamine (TEA) into a reactor; raising the temperature of the reactor to be 60 DEG C, dripping 2-bromoethanol, and controlling the reaction temperature to be less than 95 DEG C; after finishing the dripping of the 2-bromoethanol, carrying out thermal reaction in the reactor for two hours; cooling to the room temperature so as to evaporate a solvent, washing by sequentially using dicarbon monoxide (DCM), 10% hydrochloric acid, sodium bicarbonate saturated solution and water, concentrating an organic layer to a constant weight, and adding ethyl alcohol to recrystalize so as to obtain an intermediate product; adding MeOH and the intermediate product into a reactor and stirring; dripping hydrazine hydrate, and increasing the temperature to be 68 DEG C after finishing the dripping; cooling, filtering and concentrating a filter liquor, then adding chloroform, and filtering and concentrating the filter liquor; and distilling the residuum at reduced pressure so as to obtain the 2-(aminooxy)ethanol. The preparation method is simple to operate and low in cost, causes less pollution, and is high in product purity and suitable for industrial large-scale application.

Description

technical field [0001] The invention relates to a preparation method of ethanol derivatives, in particular to a preparation method of 2-(aminooxy)ethanol. Background technique [0002] 2-(aminooxy)ethanol, namely 2-(aminooxy)ethanol, is a pharmaceutical intermediate. At present, many manufacturers at home and abroad are using it as a raw material for the development of raw materials, and it has a good market prospect. The synthesis method of 2-(aminooxy)ethanol in the prior art has the defects of low reaction yield and low product purity. Contents of the invention [0003] Aiming at the shortcomings and deficiencies of the prior art, the invention provides a preparation method of 2-(aminooxy)ethanol, which is simple in operation, low in cost and less in pollution, and is suitable for large-scale industrial application. [0004] The present invention is achieved through the following technical solutions: [0005] A preparation method of 2-(aminooxy)ethanol, comprising the...

Claims

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Application Information

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IPC IPC(8): C07C239/20
Inventor 纪兴国
Owner 纪兴国
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