Method for preparing methoxyamine hydrochloride by adopting microreactor

A technology of methoxyamine hydrochloride and microreactor, which is applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical processes, etc., can solve the problem of methoxyamine hydrochloride collection The efficiency and purity are not very high, so as to achieve the effect of improving product selectivity, reducing by-products and low production cost

Active Publication Date: 2021-06-29
南京科力硕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for preparing methoxyamine hydrochloride by adopting microreactor
  • Method for preparing methoxyamine hydrochloride by adopting microreactor

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 adopting a microreactor. The method specifically comprises the steps of preparation of acetohydroxylamine, preparation of acetomethoxylamine and preparation of methoxylamine hydrochloride, wherein the preparation processes of acetohydroxylamine and acetomethoxylamine are carried out in a microreactor. Specifically, a hydroxylamine hydrochloride solution, ethyl acetate and alkali liquor are pumped into a micro-channel reaction module A and mixed in a micro-channel, then the mixture, dimethyl sulfate and alkali liquor are pumped into a micro-channel reaction module B again, collection is conducted after mixed reaction, and then the methoxylamine hydrochloride is obtained through the processes of hydrolysis, distillation, neutralization, salification, concentration and the like. Compared with the prior art, the method has the advantages that the yield of methoxyamine hydrochloride is effectively improved by utilizing the microreactor, the generation of three wastes is reduced, the reaction time is shortened, and the production cost is reduced.

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 Applications(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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