Preparation method for methoxylamine hydrochloride

A technology of methoxyamine hydrochloride and acetylmethoxyamine, which is applied in the field of preparation of methoxyamine hydrochloride, can solve the problems of safety and environmental protection risks, complicated and serious reaction processes, and achieves reduction of exhaust gas emissions and reaction conditions. Mild, stress-relieving effect of the environment

Inactive Publication Date: 2013-03-20
张家港市大伟助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process is relatively complicated, requiring the use of liquid sulfur dioxide and sodium nitrite, which is not only highly toxic but also seriously pollut

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) Dissolve 1 mol of hydroxylamine hydrochloride and 6.5 mol of potassium carbonate in 40% ethanol aqueous solution (9 mol of ethanol), add 1.8 mol of ethyl acetate, heat to 55-65°C for 2 hours, wash with water 4 times, Dry over anhydrous sodium sulfate, and recover ethanol by rotary evaporation to obtain 0.96 mol of acetaminolamine.

[0018] 2) Under the ice bath condition of -10~0℃, dissolve 0.96mol of acetohydroxylamine and 2.0mol of sodium hydroxide in 40% ethanol aqueous solution (3.0mol of ethanol), and add 1.65mol of dimethyl sulfate dropwise , react at room temperature for 3 h, filter with suction, wash the filter cake with ethanol, combine the washing liquid with the filtrate, and concentrate under reduced pressure to obtain 0.92 mol of acetomethoxylamine.

[0019] 3) Mix 0.92mol of acetomethoxamine with 50% sulfuric acid solution (the sulfuric acid is 1.3mol), and heat to 70-80°C for 3h, distill at atmospheric pressure for 1.5h, recover acetic acid, cool down ...

Embodiment 2

[0021] 1) Dissolve 2 mol of hydroxylamine hydrochloride and 15 mol of potassium carbonate in 50% ethanol aqueous solution (18 mol of ethanol), add 4.0 mol of ethyl acetate, heat to 55-65°C for 2 hours under reflux, wash with water 4 times, no Water was dried with sodium sulfate, and ethanol was recovered by rotary evaporation to obtain 1.9 mol of acetohydroxylamine.

[0022] 2) Under the condition of ice bath at -10~0℃, dissolve 1.9mol of acetohydroxylamine and 4.2mol of sodium hydroxide in 50% ethanol aqueous solution (7.0mol of ethanol), and dropwise add 3.8mol of dimethyl sulfate , reacted at room temperature for 4h, filtered with suction, washed the filter cake with ethanol, combined the washing liquid with the filtrate, and concentrated under reduced pressure to obtain 1.86 mol of acetomethoxylamine.

[0023] 3) Mix 1.86mol of acetomethoxamine with 50% sulfuric acid solution (the sulfuric acid is 2.8mol), and heat it to 70-80°C for 4 hours, distill at atmospheric pressure...

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PUM

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Abstract

The invention discloses a preparation method for methoxylamine hydrochloride, comprising the following preparation steps of: 1) preparing acetyl hydroxylamine; 2) preparing acetyl methoxyamine; and 3) preparing methoxylamine hydrochloride. The preparation method is moderate in reaction conditions, and is capable of avoiding the toxic substances such as sulfur dioxide and sodium nitrite which are used in the existing production process for methoxylamine hydrochloride, reducing the emission of waste gases such as nitric oxide, and lightening a pressure of environment.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of methoxyamine hydrochloride. Background technique [0002] Methoxyamine hydrochloride is an important chemical product and pharmaceutical intermediate, which can be used in color photography and film printing, and is widely used in the synthesis of medicine, functional dyes, low-toxicity pesticides and new herbicides. Methoxyamine hydrochloride is mainly used in the synthesis of the second-generation cephalosporin product cefuroxime, as well as the synthesis of sulfamethoxazole, ethinazole, and hydroxyurea in the aspect of medicine; it is mainly used in the synthesis of high-efficiency and low-toxicity Phenoxystrobin. With the continuous development of its application fields, the demand for methoxyamine hydrochloride at home and abroad is increasing. [0003] At present, domestic methoxyamine hydrochloride production enterprises basically use ...

Claims

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Application Information

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IPC IPC(8): C07C239/20
Inventor 龚卫良黄德周
Owner 张家港市大伟助剂有限公司
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