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A kind of method adopting microreactor to prepare methoxyamine hydrochloride

A methoxyamine hydrochloride, microreactor technology, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, organic chemistry, etc., can solve the problem that the yield and purity of methoxyamine hydrochloride are not very high. High problems, to achieve the effect of improving product selectivity, less three wastes, and low production cost

Active Publication Date: 2022-03-08
南京科力硕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, the yield and the purity of the methoxyamine hydrochloride produced by its preparation method are not very high

Method used

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  • A kind of method adopting microreactor to prepare methoxyamine hydrochloride
  • A kind of method adopting microreactor to prepare methoxyamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of embodiment 1 methoxyamine hydrochloride

[0029] according to figure 1 The connection method is used to build a microreactor and carry out the reaction:

[0030] (1) Weigh 10g of hydroxylamine hydrochloride and add it to 100mL of water and stir to obtain hydroxylamine hydrochloride solution, add 20g of ethyl acetate and 60g of 20% sodium hydroxide solution into the material tank respectively, and then pump it into the microchannel through a constant flow pump In the reaction module A, the reaction obtains solution a;

[0031] (2) 190 g of solution a, 10 g of dimethyl sulfate and 60 g of 20% sodium hydroxide solution were pumped into the microchannel reaction module B to react to obtain solution b;

[0032] (3) Take solution b out of the collection tank, add hydrochloric acid (hydrolysis step), and reflux at 65°C for 1 h; then distill under atmospheric pressure at 65°C (distillation step), and cool the solution to 40°C; add sodium hydroxide s...

Embodiment 2

[0033] The preparation method of embodiment 2 methoxyamine hydrochloride

[0034] (1) Weigh 500g of hydroxylamine hydrochloride and add it to 500mL of water and stir to obtain hydroxylamine hydrochloride solution, add 1000g of ethyl acetate and 3000g of 10% sodium hydroxide solution to the material tank respectively, and then pump it into the microchannel through a constant flow pump In the reaction module A, the reaction obtains solution a;

[0035] (2) respectively pump 5000g of solution a, 1000g of dimethyl sulfate and 3000g of 10% sodium hydroxide solution into the microchannel reaction module B to react to obtain solution b;

[0036] (3) Take out 9000g of solution b in the collection tank, add hydrochloric acid (hydrolysis step), and reflux at 65°C for 1 h; then distill under atmospheric pressure at 65°C (distillation step), and cool the solution with circulating water and ice brine to 40°C; add sodium hydroxide solution to make the pH of the solution reach about 7.0 (ne...

Embodiment 3

[0037] The preparation method of embodiment 3 methoxyamine hydrochloride

[0038] (1) Weigh 250g of hydroxylamine hydrochloride and add it into 500 mL of water and stir to obtain hydroxylamine hydrochloride solution, add 500g of ethyl acetate and 1000g of 10% sodium hydroxide solution into the material tank respectively, and then pump it into the micro In channel reaction module A, the reaction obtains solution a;

[0039](2) Pump 22500g of solution a, 500g of dimethyl sulfate and 1000g of 31% sodium hydroxide solution into the microchannel reaction module B to react to obtain solution b;

[0040] (3) Take out 3750g of solution b in the collection tank, add hydrochloric acid (hydrolysis step), and reflux at 65°C for 1 h; then distill at 65°C under atmospheric pressure (distillation step), and cool the solution with circulating water and ice brine to 40°C; add sodium hydroxide solution to make the pH of the solution reach about 7.0 (neutralization step), stir for 10 minutes; a...

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Abstract

The invention belongs to the field of synthesis of fine chemical intermediates, and discloses a method for preparing methoxyamine hydrochloride by using a microreactor. It is specifically divided into: the preparation of acetaminolamine, the preparation of acetylmethoxamine and the preparation of methoxylamine hydrochloride, wherein the preparation process of acetylhydroxylamine and acetylmethoxylamine is carried out in a microreactor. Specifically, the hydroxylamine hydrochloride solution, ethyl acetate and lye are pumped into the microchannel reaction module A, and after being mixed in the microchannel, they are pumped into the microchannel reaction module B again with dimethyl sulfate and lye, and collected after the mixed reaction. After hydrolysis, distillation, neutralization, salt formation, concentration and other processes, methoxyamine hydrochloride is obtained. Compared with the prior art, the invention effectively improves the yield of methoxyamine hydrochloride by utilizing the microreactor, reduces the generation of three wastes, shortens the reaction time and reduces the production cost.

Description

technical field [0001] The invention relates to the field of synthesis of fine chemical intermediates, in particular to a method for preparing methoxyamine hydrochloride using a microreactor. Background technique [0002] Methoxyamine hydrochloride is an important chemical raw material, which is widely used in the preparation and synthesis of low-toxic pesticides, new herbicides, medicines, and functional dyes. In the field of pesticides, methoxyamine hydrochloride is mainly used to synthesize phenoxystrobin with high efficiency and low toxicity; in the field of medicine, it is used in the synthesis of the second-generation cephalosporin product cefuroxime, as well as Synthesis of Promin, Hydroxyurea, etc. The main production sites of methoxyamine hydrochloride abroad are concentrated in India, the production technology is relatively backward, the operation safety needs to be improved, and a large amount of three wastes are likely to be generated during the preparation proc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C239/20B01J19/00
CPCC07C239/20B01J19/0093
Inventor 李泽平曹逊姜深伟顾利斌
Owner 南京科力硕生物科技有限公司
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