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Preparation method of methoxyamine hydrochloride and preparation method of N-methoxyacetamide

A technology of methoxyacetamide and methoxylamine hydrochloride, which is applied in the field of preparation of methoxylamine hydrochloride, can solve the problem of insufficient yield, insufficient purity of methoxylamine hydrochloride, and limited methoxylamine hydrochloride. Problems such as the promotion and application of hydrochloride

Pending Publication Date: 2021-05-28
ZHENGZHOU SIGMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although methoxyamine hydrochloride has high application value, the method for preparing methoxyamine hydrochloride in existing literature, or the purity of the obtained methoxyamine hydrochloride is not high enough, or the yield is not high enough, in To a certain extent, it limits the popularization and application of methoxyamine hydrochloride

Method used

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  • Preparation method of methoxyamine hydrochloride and preparation method of N-methoxyacetamide
  • Preparation method of methoxyamine hydrochloride and preparation method of N-methoxyacetamide

Examples

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Embodiment 1

[0039] The preparation method of the methoxylamine hydrochloride of the present embodiment may further comprise the steps:

[0040] 1) Add 0.10 mol of sodium bicarbonate and 3.52 mol of sodium hydroxide to 200 g of water and mix evenly to obtain a composite alkali aqueous solution (i.e. a mixed aqueous solution);

[0041] 2) Add 108g (1.44mol) acetylhydroxamic acid and 200g water to the reaction flask and mix to obtain a reaction solution. Control the temperature of the reaction solution at 10°C, add 181.6g (1.44mol) dimethyl sulfate dropwise, and simultaneously add compound Alkali aqueous solution, control the pH of the reaction system to 7.0-7.5, drop in 2 hours, and stir for 0.5h after adding dimethyl sulfate. Then dropwise add 27.2g (0.22mol) dimethyl sulfate, dropwise add aqueous solution of composite base, control reaction system pH=7.0-7.5, stir 0.5h after dropping, then dropwise add 45.4g (0.36mol) dimethyl sulfate, At the same time, the aqueous solution of compound a...

Embodiment 2

[0044] The preparation method of the methoxylamine hydrochloride of the present embodiment may further comprise the steps:

[0045] 1) Add 0.2mol of sodium bicarbonate and 2.3mol of sodium hydroxide to 200g of water and mix evenly to obtain a composite alkali aqueous solution (i.e. a mixed aqueous solution);

[0046] 2) Add 108g (1.44mol) of acetylhydroxamic acid and 252g of water into the reaction flask and mix to obtain a reaction solution. Control the temperature of the reaction solution at 20°C, add 163.4g (1.30mol) of dimethyl sulfate dropwise, and simultaneously add compound Alkaline aqueous solution, control the pH of the reaction system to 7.5-8.0, drop it in 2 hours, and stir for 0.5 h after adding dimethyl sulfate. Then continue to dropwise add 18.1g (0.14mol) of dimethyl sulfate, and dropwise add a complex alkali aqueous solution at the same time, control the pH of the reaction system=7.5-8.0, stir for 0.5h after dropping, then add dropwise 27.2g (0.22mol) of dimeth...

Embodiment 3

[0049] The preparation method of the methoxylamine hydrochloride of the present embodiment may further comprise the steps:

[0050] 1) Add 0.15 mol of sodium bicarbonate and 3.0 mol of sodium hydroxide to 200 g of water and mix evenly to obtain a composite alkali aqueous solution (i.e. a mixed aqueous solution);

[0051] 2) Add 108g (1.44mol) of acetylhydroxamic acid and 162g of water into the reaction flask and mix to obtain a reaction solution. Control the temperature of the reaction solution at 30°C, add 154.3g (1.22mol) of dimethyl sulfate dropwise, and simultaneously add the compound Alkali aqueous solution, control the pH of the reaction system to 8-9, drop after 2 hours, and stir for 0.5h after adding dimethyl sulfate. Then continue to add dropwise 9.1g (0.08mol) dimethyl sulfate, and dropwise add the aqueous solution of compound alkali to control the pH of the reaction system=8-9, stir for 0.5h after dropping, then add dropwise 18.1g (0.14mol) dimethyl sulfate , and a...

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Abstract

The invention relates to a preparation method of methoxyamine hydrochloride and a preparation method of N-methoxyacetamide, belonging to the technical field of organic synthesis. The preparation method of the methoxyamine hydrochloride comprises the following steps: 1) carrying out a methylation reaction on acetohydroxamic acid and dimethyl sulfate in water to generate N-methoxyacetamide, wherein in the process of the methylation reaction, sodium bicarbonate and sodium hydrogen salt are adopted to control the pH value of a reaction system to be 7-9, and a molar ratio of sodium bicarbonate to sodium hydroxide is (0.03-0.09): 1; and 2) preparing methoxyamine hydrochloride from N-methoxyacetamide. According to the preparation method of methoxyamine hydrochloride, composite alkali of sodium bicarbonate and sodium hydroxide is adopted in the methylation reaction process, so the conversion rate of acetohydroxamic acid can be increased, the pH value in the methylation process can be strictly controlled to be 7-9, generation of polymethylation impurities (O,N-dimethylhydroxylamine hydrochloride) is reduced, and the yield of N-methoxyacetamide is improved.

Description

technical field [0001] The invention relates to a preparation method of methoxyamine hydrochloride and a preparation method of N-methoxyacetamide, belonging to the technical field of organic synthesis. Background technique [0002] Methoxyamine hydrochloride (molecular formula is CH 3 ONH 2 ·HCl) is an important chemical raw material for the production of antibiotics such as cefuroxime acid (ester) and phenoxystrobin fungicides; Maintain or restore arterial pressure, especially for blood pressure reduction caused by spinal anesthesia. [0003] Although methoxyamine hydrochloride has high application value, the method for preparing methoxyamine hydrochloride in existing literature, or the purity of the obtained methoxyamine hydrochloride is not high enough, or the yield is not high enough, in To a certain extent, the popularization and application of methoxyamine hydrochloride is limited. Contents of the invention [0004] The purpose of this invention is to provide a k...

Claims

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Application Information

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IPC IPC(8): C07C239/20C07C259/06
CPCC07C239/20C07C259/06
Inventor 冯云霞王英豪张高锋申丽坤杨勇
Owner ZHENGZHOU SIGMA CHEM
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