Synthetic method of furan ammonium salt

A technology of furan ammonium salt and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of low yield, and achieve the effects of high yield, reduced production cost, and reduced ammonia nitrogen content

Active Publication Date: 2021-02-02
YIYUAN XINQUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of the direct reaction of 2-oxo-2-furyl acetic acid and methoxyamine is still lower than that of the existing process, and still needs to be improved.

Method used

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  • Synthetic method of furan ammonium salt
  • Synthetic method of furan ammonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Stir 180g of purified water and 18g of sulfuric acid evenly, add 1.1g of copper chloride, stir evenly, add 20g of acetylfuran, control the temperature at 52±2°C, slowly inject 23g of methyl nitrite, control the aeration time at 1 hour, and the aeration is completed After the reaction was incubated for 3 hours, after the reaction was completed, liquid caustic soda was added to adjust its pH value to 4, 1 g of activated carbon was added to the reaction solution, stirred for 30 minutes and filtered, after the filtration was completed, 200 mL of dichloromethane was added to extract twice, and the organic phase was combined. Slowly add a saturated ethanol solution of ammonia gas (a saturated ethanol solution of ammonia gas at -5°C) dropwise to the organic phase to adjust the pH to 8, keep stirring at 0°C for 30 min, and filter with suction to obtain a light yellow solid with a volume ratio of two Methyl chloride:ethanol=6:1 mixed solution 200mL soaks and washes the filter cak...

Embodiment 2

[0026] Stir 180g of purified water and 20g of sulfuric acid evenly, add 1.3g of ferric chloride, stir evenly, add 20g of acetylfuran, control the temperature at 55-60°C, slowly introduce 23g of methyl nitrite, control the aeration time at 2 hours, and the aeration is completed Rear insulation reaction 6 hours, add liquid caustic soda to adjust its pH value to 6 after the completion of the reaction, add 1g gac to the reaction solution, stir and filter for 30 minutes,

[0027] After filtration, add 200mL dichloromethane to extract twice, combine the organic phases, and slowly add a saturated ethanol solution of ammonia gas (-5°C ammonia ethanol saturated solution) to the organic phase to adjust the pH to 8. Lower heat preservation and stirring for 30min, suction filtration, to obtain a light yellow solid, with a volume ratio of dichloromethane: ethanol=6:1 mixed solution 200mL bubble wash filter cake, to obtain a white powdery solid, i.e. furan ammonium salt 22.1g, yield It is 6...

Embodiment 3

[0029] Stir 180g of purified water and 17g of sulfuric acid evenly, add 1.25g of copper chloride, stir evenly, add 20g of acetylfuran, control the temperature at 55-60°C, slowly introduce 23g of methyl nitrite, control the aeration time at 5 hours, and the aeration is completed After the reaction was incubated for 5 hours, after the reaction was completed, ammonia water was added to adjust its pH value to 5, and 1 g of activated carbon was added to the reaction solution, stirred for 30 minutes and filtered.

[0030] After filtration, add 200mL dichloromethane to extract twice, combine the organic phases, and slowly add a saturated ethanol solution of ammonia gas (-5°C ammonia ethanol saturated solution) to the organic phase to adjust the pH to 8. Lower heat preservation and stirring for 30min, suction filtration, to obtain a light yellow solid, with a volume ratio of dichloromethane: ethanol=6:1 mixed solution 200mL bubble wash filter cake, to obtain a white powdery solid, i.e....

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Abstract

The invention particularly relates to a synthetic method of furan ammonium salt, and belongs to the technical field of synthesis of medical intermediates. The synthesis method of the furan ammonium salt comprises the following steps: under the catalytic action of a metal salt, reacting acetylfuran with methyl nitrite to obtain 2-imino-2-furan acetic acid, introducing ammonia gas, and carrying outafter-treatment to obtain the furan ammonium salt. The synthesis method of the furan ammonium salt is simple and feasible, reduces the production cost, improves the product yield, is safe and environment-friendly, and has remarkable economic benefits and environment-friendly benefits.

Description

technical field [0001] The invention specifically relates to a method for synthesizing furan ammonium salt, and belongs to the technical field of synthesis of pharmaceutical intermediates. Background technique [0002] Cis-furan ammonium salt is a key intermediate for the synthesis of broad-spectrum antibiotic cefuroxime axetil (sodium). With the rapid increase in demand for cefuroxime axetil (sodium) in domestic and foreign markets, the market demand for cis-furan ammonium salt has also increased significantly. promote. [0003] The structural formula of cis furan ammonium salt is as follows: [0004] [0005] The most general preparation method of furan ammonium salt industrial production comprises the following steps: [0006] 2-Oxo-2-furyl acetic acid, water, and adjust the pH value with inorganic acid, then add methoxyamine aqueous solution or its hydrochloride aqueous solution; heat preservation reaction, the reaction process is controlled by inorganic alkali and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/54
CPCC07D307/54
Inventor 吕敦生常明珠周磊张立明马祥云
Owner YIYUAN XINQUAN CHEM
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