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Method for preparing furan ammonium salt with high selectivity

A furan ammonium salt, high selectivity technology, applied in the direction of organic chemistry and the like, can solve the problems of harsh reaction conditions, low furan ammonium salt yield, low 2-acetylfuran conversion rate, etc. in the furan ammonium salt preparation process, and achieves low price. , the effect of improving oxidation conversion, improving yield and purity

Active Publication Date: 2021-06-01
安徽金轩科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve problems such as low conversion rate of raw material 2-acetylfuran in the prior art, low furan ammonium salt yield, harsh reaction conditions of furan ammonium salt preparation process, and a kind of highly selective preparation of furan ammonium proposed salt method

Method used

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Effect test

Embodiment 1

[0023] A kind of method that the present invention proposes to prepare furan ammonium salt with high selectivity comprises the following steps:

[0024] S1. Oxidation process: add water and acidic solution into the oxidation kettle to obtain a mixed solvent with a pH value of 2.8, add 2-acetylfuran while stirring at a speed of 200r / min, raise the temperature to 40°C, continue stirring and drop the oxidant, After the dropwise addition, the insulation reaction was carried out for 2 hours. After the reaction was completed, 2-oxo-2-furan acetic acid was obtained by extraction with dichloromethane, wherein the acidic solution was obtained by compounding hydrochloric acid and phosphoric acid with a mass ratio of 1:1, and the oxidant was obtained by mass ratio It is obtained by compounding peracetic acid, sodium perborate and water at a ratio of 1:2:4.5, and the addition amount of the oxidizing agent is 3% of the total amount of 2-acetylfuran;

[0025] S2. Oximation process: Add the ...

Embodiment 2

[0028] A kind of method that the present invention proposes to prepare furan ammonium salt with high selectivity comprises the following steps:

[0029] S1. Oxidation process: Add water and acidic solution into the oxidation kettle to obtain a mixed solvent with a pH value of 3.5, add 2-acetylfuran while stirring at a speed of 400r / min, raise the temperature to 45°C, continue stirring and drop the oxidant, After the dropwise addition, the insulation reaction was carried out for 2.5 hours. After the reaction was completed, 2-oxo-2-furan acetic acid was obtained by extraction with dichloromethane. The acidic solution was obtained by compounding hydrochloric acid and phosphoric acid with a mass ratio of 2:1. It is obtained by compounding peracetic acid, sodium perborate and water with a ratio of 1:2.5:5.8, and the addition amount of oxidant is 5% of the total amount of 2-acetylfuran;

[0030] S2. Oximation process: add the 2-oxo-2-furanacetic acid prepared in step S1 into the oxi...

Embodiment 3

[0033] A kind of method that the present invention proposes to prepare furan ammonium salt with high selectivity comprises the following steps:

[0034] S1. Oxidation process: add water and acidic solution into the oxidation kettle to obtain a mixed solvent with a pH value of 4.5, add 2-acetylfuran while stirring at a speed of 600r / min, raise the temperature to 50°C, continue stirring and drop the oxidant, After the dropwise addition, the insulation reaction was carried out for 3 hours. After the reaction was completed, 2-oxo-2-furan acetic acid was obtained by extraction with dichloromethane, wherein the acidic solution was obtained by compounding hydrochloric acid and phosphoric acid with a mass ratio of 3:1, and the oxidant was obtained by mass ratio It is obtained by compounding peracetic acid, sodium perborate and water at a ratio of 1:3:7, and the amount of oxidant added is 8% of the total amount of 2-acetylfuran;

[0035] S2. Oximation process: Add the 2-oxo-2-furanacet...

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Abstract

The invention belongs to the technical field of preparation of medical intermediates, particularly relates to a method for preparing furan ammonium salt with high selectivity, and solves the problems of low conversion rate of a raw material 2-acetylfuran, low yield of furan ammonium salt, harsh reaction conditions of a furan ammonium salt preparation process and the like in the prior art. The method comprises the following steps: adding water, an acidic solution and 2-acetylfuran into an oxidation kettle, heating, dropwise adding an oxidant, and reacting to obtain 2-oxo-2-furanacetic acid; cooling 2-oxo-2-furanacetic acid, and then adding methoxyamine to react, so as to obtain 2-methoxyamine-2-furanacetic acid; adding methanol an ammoniation salifying kettle, adding 2-methoxyamine-2-furanacetic acid, introducing ammonia gas for a reaction, and obtaining the furan ammonium salt. The synthesis raw materials are low in price and easy to obtain, the preparation process is mild in reaction condition, safe and environmentally friendly, the yield and purity of the furan ammonium salt product are improved, and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical intermediates, in particular to a method for preparing ammonium furan with high selectivity. Background technique [0002] Cephalosporin antibiotics are the most widely used anti-infective drugs in clinical application in recent years. Cefuroxime (including cefuroxime sodium and cefuroxime axetil), as a second-generation cephalosporin, was originally researched and developed by the British Glaxo Company. It has broad-spectrum antibacterial activity and low toxic and side effects. The resistance of positive bacteria is similar to that of the first-generation cephalosporins, and its sensitivity rate is over 95%. However, the resistance to Gram-negative bacteria is greatly enhanced, such as Haemophilus influenzae, Escherichia coli, Salmonella, mirabilis Bacteria, meningococcus, etc. are very sensitive, and are basically non-toxic to the kidney. Clinically, it is mainly used for...

Claims

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Application Information

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IPC IPC(8): C07D307/58
CPCC07D307/58
Inventor 程光锦孙多龙胡坤伏忠祥
Owner 安徽金轩科技有限公司
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