Method for producing furan ammonium salt by using furoic acid

A technology of furan ammonium salt and furan formic acid, applied in directions such as organic chemistry, can solve problems such as waste of alcohol and ammonia raw materials, unfavorable large-scale production, increased production input, etc., and achieves good product quality, safe and reliable production process, and reduced resources. wasteful effect

Inactive Publication Date: 2012-07-04
湖北楚阳科技股份有限公司
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  • Abstract
  • Description
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Problems solved by technology

Although the process is relatively stable, in the oximation process, due to the pH, temperature and reaction time, it will have a huge impact on product indicators and yield, and will increase production input and cost, which is not conducive to large-scale production.
At the same time, when pH is adjusted in the process of forming ammonium, the increase of alcohol ammonia also causes waste of raw materials, which is not conducive to production

Method used

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  • Method for producing furan ammonium salt by using furoic acid

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Embodiment 1

[0017] Below in conjunction with accompanying drawing, the present invention is described in further detail:

[0018] A preparation method utilizing furanic acid to produce furan ammonium salt, the steps are:

[0019] (1) Chlorination: 112kg of furanic acid (purchased) as a raw material and 500kg of dichloromethane as a solvent are put into a glass-lined reaction kettle, the stirring and heating system is turned on, and the temperature is controlled at 10 or 20 or 30 or 35 or 45 or 52 or 58 or 60 ℃, add 137.5 kg (1000 mol) of chlorinating agent phosphorus trichloride. React for 5 or 6 or 7 or 8 or 9 or 10 hours, reduce the pressure to -0.08MPa and recover dichloromethane. Then the product furoyl chloride was distilled off under reduced pressure at -0.095Mpa at 50°C to obtain about 125kg of the product.

[0020] (2) Cyanide: Add 55kg (1000mol) of sodium cyanide (1000mol) of sodium cyanide and 120kg of acetonitrile into the reactor and stir to cool down at -10 or -15 or -1...

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Abstract

The invention discloses a method for producing a furan ammonium salt by using furoic acid. The method comprises the following steps of: (1) chlorination: putting furoic acid and chlorohydrocarbon solvent into an enameled glass reaction kettle, controlling temperature and time, and obtaining a furoyl chloride product; (2) cyanation: putting the furoyl chloride and sodium cyanide into the reaction kettle, stirring, preserving heat, reducing pressure, and reclaiming the solvent to obtain a furoyl nitrile product; (3) hydrolysis: heating the furoyl nitrile and hydrochloric acid, and obtaining furan ketone acid after the reaction is finished; (4) condensation: adding ethyl acetate extract of the furan ketone acid serving as the hydrolysis product into the reaction kettle, dropping methoxyamineto perform room temperature reaction with the hydrolysis product, and demixing, wherein the oil layer is used for ammoniation reaction; and (5) ammoniation: introducing ammonia gas into the oil layerreactant, controlling the temperature, stirring, finishing gas introduction, centrifuging, and drying to obtain the furan ammonium salt. The method is simple and convenient, is convenient to operate,reduces the production cost, improves the yield, makes full use of raw materials, and is safe and reliable in the production process.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis of cefuroxime axetil and cefuroxime sodium, and more specifically relates to a preparation method for synthesizing furan ammonium salt, which is suitable for synthesizing second-generation cephalosporin intermediates using furancarboxylic acid as a raw material. Background technique [0002] At present, the cephalosporin antibiotics cefuroxime sodium and cefuroxime axetil have good curative effects, and the dosage of these drugs is increasing, and furan ammonium salt is a new type of pharmaceutical intermediate, and it is also the second generation of cephalosporins. The key intermediate of furocin, the domestic synthesis technology of this product is not yet very mature, and the output is still very low. Ammonium furan salt is very promising in the current market, but it cannot meet the domestic market demand in terms of output and quality. Therefore, there is a lot of room fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/54
Inventor 陈涛郭海涛李祯邓德忠邓德政黄长富王鹏
Owner 湖北楚阳科技股份有限公司
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