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Method for synthesizing methoxyamine hydrochloride

A technology of methoxyamine hydrochloride and mixed solution, which is applied in chemical instruments and methods, chemical/physical/physical chemical fixed reactors, chemical/physical/physical chemical processes, etc., can solve problems such as cumbersome operation, and achieve The effect of uniform reaction, low emission, and reduced investment cost

Pending Publication Date: 2021-12-07
宁波四明化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional reaction kettle generally includes a kettle body and a kettle cover. After the reactants are mixed and reacted in the kettle body, some of them will inevitably remain on the side wall of the kettle body, and the residues on the side wall of the kettle body are generally removed by regular cleaning. , the kettle cover needs to be removed from the kettle body when cleaning, the operation is cumbersome and needs to be improved

Method used

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  • Method for synthesizing methoxyamine hydrochloride
  • Method for synthesizing methoxyamine hydrochloride
  • Method for synthesizing methoxyamine hydrochloride

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Embodiment Construction

[0041] The following is attached Figure 1-4 The application is described in further detail.

[0042] The embodiment of the present application discloses a method for synthesizing methoxyamine hydrochloride. refer to figure 1 , figure 2 , the method for synthesizing methoxyamine hydrochloride comprises the steps:

[0043] S1. Add water and sodium hydroxide to reactor 1, stir and dissolve at room temperature, then add butanone oxime and a phase transfer catalyst, wherein the phase transfer catalyst is PEG500;

[0044] S2. Cool the inside of the reactor 1 to 0-15°C, specifically, to 5°C, and add a methylating reagent to the reactor 1, wherein the methylating reagent is dimethyl sulfate;

[0045] S3. After the addition is completed, react at a temperature of 10°C for 4 hours, then cool to below 5°C and stand to separate layers to obtain an organic layer and a water layer, distill the water layer and collect the distillate, then combine the oil layer and the distillate, and t...

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Abstract

The invention relates to the technical field of compound synthesis methods, and discloses a method for synthesizing methoxyamine hydrochloride. The method comprises the following steps: adding water, sodium hydroxide, diacetylmonoxime and a phase transfer catalyst into a reaction kettle; after cooling, adding a methylation reagent; conducting standing for layering to obtain an organic layer, a water layer and a distilled water layer, collecting distillate, combining an oil layer and the distillate, and adding hydrochloric acid for mixing to obtain a mixed solution; feeding and rectifying the mixed solution from the middle of a rectifying column, recovering butanone and methanol at the top of the column, recovering a methoxyamine hydrochloride solution at the bottom of the column, and carrying out evaporating and dehydrating to obtain a concentrated solution; and cleaning a reaction kettle, wherein a stirring mechanism and a cleaning mechanism are arranged in the reaction kettle, the cleaning mechanism comprises a scraping plate, a spraying pipe, a lifting assembly and a rotating assembly, a water inlet pipe and a cleaning nozzle are connected to the spraying pipe, the reaction kettle comprises a kettle body and a kettle cover, the water outlet end of the cleaning nozzle faces the side wall of the kettle body, and the scraping plate is attached to the side wall of the kettle body. The method has the effect of conveniently cleaning residues on the side wall of the kettle body.

Description

technical field [0001] The present application relates to the technical field of compound synthesis methods, in particular to a method for synthesizing methoxyamine hydrochloride. Background technique [0002] Methoxyamine hydrochloride is an important chemical product and pharmaceutical intermediate, widely used in color photography and film printing, as a reducing agent in the organic synthesis industry to prepare oximes, and in the production of sulfamethoxazole, ethinoxazole, and hydroxyurea in medicine. , Cefuroxime, etc. [0003] As an important equipment in the chemical synthesis process, the reaction kettle is one of the necessary equipment in the synthesis process of methoxyamine hydrochloride, and its cleanliness directly affects the quality of the product. The traditional reaction kettle generally includes a kettle body and a kettle cover. After the reactants are mixed and reacted in the kettle body, some of them will inevitably remain on the side wall of the ket...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/20B01J19/18B01J19/00
CPCC07C239/20B01J19/0006B01J19/002B01J19/0053B01J19/18B01J19/0066
Inventor 王晓永方前军尚鹏飞李亚东
Owner 宁波四明化工有限公司
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