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Method of using ketoxime ether for preparation of alkoxyl amine hydrochloride and alkoxyl amine hydrochloride preparation method

A technology of hydrocarbyloxyamine hydrochloride and ketoxime ether, which is applied in the field of preparing hydrocarbyloxyamine hydrochloride and hydrocarbyloxyamine hydrochloride from ketoxime ether, and can solve the operation danger, yield and low cost. problems such as low yield, to achieve the effect of reducing production costs

Active Publication Date: 2013-02-06
宁波四明化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to provide a new method for preparing alkoxyamine hydrochloride from ketoxime ether in order to overcome the disadvantages of operation risk and low yield and yield in the existing preparation method of alkoxyamine hydrochloride. salt method

Method used

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  • Method of using ketoxime ether for preparation of alkoxyl amine hydrochloride and alkoxyl amine hydrochloride preparation method
  • Method of using ketoxime ether for preparation of alkoxyl amine hydrochloride and alkoxyl amine hydrochloride preparation method
  • Method of using ketoxime ether for preparation of alkoxyl amine hydrochloride and alkoxyl amine hydrochloride preparation method

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preparation example Construction

[0031] According to a second aspect of the present invention, the present invention also provides a method for preparing alkoxyamine hydrochloride, the method comprising the following steps:

[0032] (1) Under the reaction conditions of ketoammoxime reaction, in the presence of a titanium silicon molecular sieve catalyst, acetone or butanone, hydrogen peroxide and ammonia dissolved in an organic solvent are fed into the reactor for contact reaction to obtain acetone oxime or butanone oxime, wherein the molar ratio of hydrogen peroxide to acetone or butanone is 1-1.3;

[0033] (2) Under the substitution reaction conditions, the acetone oxime or butanone oxime obtained in step (1) is contacted with a halogenated hydrocarbon, and the acetone oxime ether or butanone oxime ether is separated from the product obtained after the contact reaction ;

[0034] (3) According to the method for preparing alkoxyamine hydrochloride from ketoxime ether described above, the acetone oxime ether...

Embodiment approach

[0056] According to the method provided by the present invention, as can be seen from the above reaction formula (1), another product (product except alkoxyamine hydrochloride) of step (3) is acetone or butanone, and in In the catalytic rectification process, acetone or butanone is discharged from the top of the rectification tower; in addition, since there is no additional organic solvent in the step (3), the acetone or butanone in the overhead distillate passes through or not After concentration, it can be directly recycled for use in step (1), and the presence of a small amount of HCl in the overhead distillate also helps to stabilize hydrogen peroxide in step (1). Therefore, according to another preferred embodiment of the present invention, the method further includes: recycling the overhead distillate of the rectification tower to be used as at least part of the acetone or butane in step (1) after being concentrated or not. ketone. In this preferred embodiment, the acet...

Embodiment 1

[0061] This example is used to illustrate the method for preparing alkoxyamine hydrochloride from ketoxime ether of the present invention and.

[0062] (1) Preparation of acetone oxime

[0063] Add 1.2g of TS-1 molecular sieve catalyst (prepared according to the method of Example 1 in CN1301599A), 11.6g of acetone, 35g of tert-butanol and 22g of ammonia water with a concentration of 25% by weight into a 200ml reactor. The mixture in the reactor was fully mixed, the reactor was sealed, and the reaction temperature was controlled at 80°C. Continuously add 26 g of hydrogen peroxide with a concentration of 30% by weight with a micro feed pump. Hydrogen peroxide was continuously pumped in for 2 hours, and the reaction was continued for 1 hour. After the reaction, the solid catalyst was separated from the mixed liquid, and the resulting liquid was cooled to room temperature, extracted 3 times with tetrachloroethylene, and the extract layer liquid was combined, then subjected to va...

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Abstract

The invention relates to a method of using ketoxime ether for preparation of alkoxyl amine hydrochloride. The method includes: continuously injecting acetoxime ether or diacetylmonoxime ether into a rectifying tower from a first feeding port, continuously injecting hydrochloric aqueous solution into the rectifying tower from a second feeding port, and separating out alkoxyl amine hydrochloride from tower bottom solution of the rectifying tower, wherein the number of plates or the number D1 of theoretical plates between the first feeding port and the tower bottom and the number of plates or the number D2 of theoretical plates between the second feeding port and the tower bottom respectively account for 30-80% of the total number of plates or the number of theoretical plates of the rectifying tower, and D1 is smaller thanD2. According to the method, extra organic solvents are not needed while target products can be obtained with high purity and high yield as reaction and separation are integrated, and steps for independent separation are reduced, so that production cost can be reduced.

Description

technical field [0001] The invention relates to a method for preparing alkoxyamine hydrochloride from ketoxime ether, and a preparation method for alkoxyamine hydrochloride. Background technique [0002] Hydroxyl amine hydrochloride, also known as O-substituted hydrocarbyl hydroxylamine hydrochloride, its general formula is H 2 NOR 1 HCl, where R 1 can be C 1 -C 6 Alkyl, C 2 -C 6 Alkenyl, C 7 -C 13 Aryl groups and halides of these groups (halogen can be, for example, Br, Cl, etc.). [0003] Alkoxylamine hydrochloride is a class of widely used and expensive organic synthesis intermediates. This type of compound can be used as an alkoxyamination reagent to introduce alkoxylamine groups into organic synthesis and new drug production. Ketone compounds (especially steroids); can be used as intermediates in the production of drug cefuroxime side chains and pesticides such as benzotrione, clethodim, sethoxydim and other herbicides, and can also be used as new medicines and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/38C07C249/12
Inventor 林勇罗署李玲叶长燊邱挺
Owner 宁波四明化工有限公司
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