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Synthesis method and device of ethyl 4-chloro-2-methoxyiminoacetoacetate

A technology of ethyl methoxyiminoacetoacetate and synthesis method, applied in organic chemistry, oxime preparation, etc., can solve the problems of cumbersome post-treatment, high production cost, cumbersome waste water treatment, etc., to speed up the reaction speed and improve the utilization efficiency, improving reaction selectivity and safety

Active Publication Date: 2020-11-13
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technical solution has the problem of cumbersome post-processing, because the reaction requires a nitrogen-containing basic catalyst, and after the reaction, operations such as washing with water are performed, and the waste water treatment is cumbersome, resulting in high production costs.

Method used

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  • Synthesis method and device of ethyl 4-chloro-2-methoxyiminoacetoacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1500kg (7.36kmol) of methanol solution 1500kg (7.36kmol) of 85% ethyl 2-methoxyiminoacetoacetate that has absorbed the reaction tail gas is added in the reactor, controlled by the DSC program, and the total amount of liquid chlorine feeding is controlled by the regulating valve It is 575kg (8.1kmol). In the first hour, 35% of the total liquid chlorine was introduced, and the temperature control was controlled at 28-30°C; in the second hour, 35% of the liquid chlorine was introduced, and the temperature was controlled at 25-27°C; 20%, the temperature is controlled at 23-25°C; in the fourth hour, 10% of the total liquid chlorine is introduced, and the temperature is controlled at 20-22°C. After the feed was completed, heat preservation and degassing for 4 hours to obtain ethyl 4-chloro-2-methoxyiminoacetoacetate, which was directly used in the next reaction without recovering the solvent. The liquid phase component content is 91.5%, and the yield is 92.3%. The hydrogen ...

Embodiment 2

[0036] Add 1600kg (7.39kmol) of ethanol solution 1600kg (7.39kmol) of 80% ethyl 2-methoxyiminoacetoacetate that has absorbed the reaction tail gas into the reactor, control the total amount of liquid chlorine through the control valve through the DSC program control It is 525kg (7.39kmol). In the first hour, 35% of the total liquid chlorine is fed, and the temperature control is controlled at 28-30°C; in the second hour, 30% of the liquid chlorine is fed, and the temperature is controlled at 25-27°C; 20%, the temperature is controlled at 23-25°C; in the fourth hour, 15% of the total liquid chlorine is introduced, and the temperature is controlled at 20-22°C. After the feeding, heat preservation and degassing for 3 hours to obtain ethyl 4-chloro-2-methoxyiminoacetoacetate with a liquid phase component content of 89.5% and a yield of 90.1%. The hydrogen chloride and excess chlorine gas produced by the reaction are absorbed by the solution of ethyl 2-methoxyiminoacetoacetate and...

Embodiment 3

[0038] 1600kg (7.39kmol) of ethanol solution 1600kg (7.39kmol) of 80% ethyl 2-methoxyiminoacetoacetate that has absorbed the tail gas of the reaction is added in the reactor, controlled by the DSC program, and the total amount of liquid chlorine feeding is controlled by the regulating valve It is 629kg (8.86kmol). In the first hour, 30% of the total liquid chlorine is fed, and the temperature control is controlled at 28-30°C; in the second hour, 30% of the liquid chlorine is fed, and the temperature is controlled at 25-27°C; in the third hour, 30% of the total liquid chlorine is fed. 20%, the temperature is controlled at 23-25°C; in the fourth hour, 20% of the total liquid chlorine is introduced, and the temperature is controlled at 20-22°C. After the feeding, heat preservation and degassing for 4 hours to obtain ethyl 4-chloro-2-methoxyiminoacetoacetate with a liquid phase component content of 90.4% and a yield of 91.5%. The hydrogen chloride and excess chlorine gas produced...

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Abstract

The invention relates to a synthesis method and device of ethyl 4-chloro-2-methoxyiminoacetoacetate, and the synthesis method comprises the following steps: S1, an ethyl 2-methoxyiminoacetoacetate solution absorbing reaction tail gas is added into a reaction kettle for reaction, and in the reaction process, the reaction temperature is reduced in a gradient manner while reducing of the introductionflow of chlorine gas in a gradient manner; and S2, a reaction product is subjected to heat preservation and degassing, the ethyl 4-chloro-2-methoxyiminoacetoacetate is obtained, and the removed gas is introduced into the ethyl 2-methoxyiminoacetoacetate solution and reused for the reaction in the step S1. Compared with the prior art, the synthesis method has the advantages that the reaction timecan be shortened, the utilization rate of chlorine can be increased, polychlorides can be controlled, the reaction selectivity can be improved, and finally, the cost can be obviously reduced.

Description

technical field [0001] The invention relates to the field of organic synthesis of pharmaceutical intermediates, in particular to a method and device for synthesizing ethyl 4-chloro-2-methoxyiminoacetoacetate. Background technique [0002] Aptivalic acid is an important pharmaceutical intermediate with high added value, mainly used in the synthesis of the third generation cephalosporin antibiotics. 4-Chloro-2-methoxyiminoacetoacetate ethyl is the key intermediate. There are many documents or patent reports on the synthesis of ethyl 4-chloro-2-methoxyiminoacetoacetate. The following is the mainstream synthetic reaction equation of ethyl 4-chloro-2-methoxyiminoacetoacetate: [0003] [0004] At present, the main technical problems in the synthesis process are: there is a bottleneck in the yield, the cost of raw materials is high, the reaction time is long, and the post-treatment process is cumbersome, which makes it difficult to reduce the overall production cost. [0005...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/36C07C249/12
CPCC07C249/12C07C251/36
Inventor 王朝阳毛海舫刘吉波李金海江海波李宁李鹏章平毅姚跃良郁士礼靳苗苗袁嘉成李箫磊芮姣袁平
Owner SHANGHAI INST OF TECH
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