Method for preparing 2-oxo-2-furyl acetic acid by using continuous flow micro-channel reactor

A technology of microchannel reactor and channel reactor, which is applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical processes, etc., and can solve the problem of low yield and pollution discharge of "three wastes" Large and other problems, to achieve high purity, improve safety and environmental protection, and reduce costs

Active Publication Date: 2019-12-31
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the invention is to solve the problems of low yield and large discharge of "three wastes" pollution in the synthesis of 2-oxo-2-furyl acetic acid in the prior art, and provides a method for preparing 2 -Oxo-2-furylacetic acid method

Method used

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  • Method for preparing 2-oxo-2-furyl acetic acid by using continuous flow micro-channel reactor
  • Method for preparing 2-oxo-2-furyl acetic acid by using continuous flow micro-channel reactor
  • Method for preparing 2-oxo-2-furyl acetic acid by using continuous flow micro-channel reactor

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Experimental program
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Effect test

Embodiment 1

[0036] 27.5g of 2-acetylfuran was dissolved in 150mL of 68% nitric acid to configure reaction solution 1, then 17.3g of sodium nitrite and 0.43g of toluenesulfonic acid (1% mol) were dissolved in 150mL of water, The molar ratio of the reaction solution 2, 2-acetylfuran and sodium nitrite is 1:1; the reaction solution 1 is poured into the cooling tower A, the reaction solution 2 is poured into the cooling tower B, and the temperature of the cooling tower is set to 5°C; after the pre-cooling is completed, use different metering pumps to pump the reaction solution 1 and the reaction solution 2 into the feed port of the continuous flow microchannel reactor, set the flow rate of the metering pump to be 5mL / min, and the microchannel reaction The temperature of the reactor is set at 60°C, and the pressure is about 1.55Mpa. After all the reaction liquid passes through the microchannel reactor, the product solution collected at the outlet is pumped into the extraction tower, and the ext...

Embodiment 2

[0038] 27.5g of 2-acetylfuran was dissolved in 150mL of 68% nitric acid to configure reaction solution 1, then 34.6g of sodium nitrite and 0.43g of toluenesulfonic acid (1% mol) were dissolved in 150mL of water, The molar ratio of the reaction solution 2, 2-acetylfuran and sodium nitrite is 1:2; the reaction solution 1 is poured into the cooling tower A, the reaction solution 2 is poured into the cooling tower B, and the temperature of the cooling tower is set to 5°C; after the pre-cooling is completed, use different metering pumps to pump the reaction solution 1 and reaction solution 2 into the feed port of the continuous flow microchannel reactor, set the flow rate of the metering pump to be 5mL / min, and the microchannel reaction The temperature of the reactor is set at 60°C, and the pressure is about 1.6Mpa. After all the reaction liquid passes through the microchannel reactor, the product solution collected at the outlet is pumped into the extraction tower, and the extracti...

Embodiment 3

[0040]27.5g of 2-acetylfuran was dissolved in 150mL of 68% nitric acid to configure reaction solution 1, then 51.9g of sodium nitrite and 0.43g of toluenesulfonic acid (1% mol) were dissolved in 150mL of water, Configure the reaction solution 2, the molar ratio of 2-acetylfuran and sodium nitrite is 1:3, pour the reaction solution 1 into the cooling tower A, and pour the reaction solution 2 into the cooling tower B, set the temperature of the cooling tower to 5 °C; after the pre-cooling is completed, use different metering pumps to pump the reaction solution 1 and reaction solution 2 into the feed port of the continuous flow microchannel reactor, set the flow rate of the metering pump to be 5mL / min, and the microchannel reactor The temperature is set at 60°C and the pressure is about 1.7Mpa. After all the reaction liquid passes through the microchannel reactor, the product solution collected at the outlet is pumped into the extraction tower. The extraction agent is 600mL of eth...

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Abstract

The invention discloses a method for preparing 2-oxo-2-furyl acetic acid by using a continuous flow micro-channel reactor. The method specifically comprises the following steps: respectively pumping anitric acid solution of 2-acetylfuran treated at low temperature and a mixed solution of sodium nitrite and methylbenzenesulfonic acid into a mixed type continuous flow micro-channel reactor by usinga metering pump for reaction, and finally extracting and recrystallizing an obtained reaction solution to obtain a finished product. Compared with the prior art, the method disclosed by the inventionpossesses following advantages: operation is simple, reaction steps are few, methylbenzenesulfonic acid is used as the catalyst, the yield of the finished product is high, no three-waste pollution isgenerated, and continuous large-scale production operation can be realized.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing 2-oxo-2-furyl acetic acid using a continuous flow microchannel reactor. Background technique [0002] 2-oxo-2-furyl acetic acid is an important pharmaceutical intermediate, which is mainly used for the synthesis of cefuroxime. Cefuroxime is a broad-spectrum antibacterial drug, which belongs to the second-generation cephalosporin and has a wide range of applications. [0003] At present, the synthesis of 2-oxo-2-furyl acetic acid mainly has the following approaches: [0004] (1) Using 2-acetylfuran as a raw material, 2-oxo-2-furyl acetic acid is obtained through condensation and oxidation; [0005] (2) Using 2-furyl acetic acid as a raw material, 2-oxo-2-furyl acetic acid is prepared through halogenation, cyanation, hydrolysis, etc.; [0006] (3) Using 2-acetylfuran as a raw material, 2-oxo-2-furyl acetic acid is obtained through oxim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/54B01J19/00
CPCC07D307/54B01J19/0093
Inventor 孙伯旺张雨晨张雨陈方慧顾地海
Owner SOUTHEAST UNIV
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