Method for recycling furan ammonium salt from furan ammonium salt waste liquid

A furan ammonium salt and waste liquid technology, applied in the direction of organic chemistry and the like, can solve the problems of high price, a large amount of waste gas, complicated process, etc., and achieve the effects of improving recovery yield, reducing environmental protection pressure, and simple steps

Active Publication Date: 2017-08-04
四平市精细化学品有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain furan ammonium salt, there are many problems: firstly, in the process of using sodium nitrite to oxidize and prepare furanone acid, a large amount of exhaust gases such as nitric oxide and nitrogen dioxide that seriously pollute the environment will be produced; secondly , in the oximation process of further converting ketoacids into furan ammonium salts, it is necessary to continue to use expensive methoxyamine, and in this process, trans-furan ammonium salts will still inevitably be produced; the process is complicated, The yield is low, which increases the cost of the recycling process
Although the yield of this method is higher and the process is relatively simple, it needs to use a medium-high pressure mercury lamp and a photochemical reactor, and the reaction temperature is not easy to control; in addition, a large amount of solvent needs to be added to the reactor, which increases the cost. Restricting its application in industrial production, it is a problem to be solved to develop a synthetic route that is cheap, environmentally friendly, easy to operate, and suitable for industrial production

Method used

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  • Method for recycling furan ammonium salt from furan ammonium salt waste liquid
  • Method for recycling furan ammonium salt from furan ammonium salt waste liquid
  • Method for recycling furan ammonium salt from furan ammonium salt waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Weigh 500g of furan ammonium salt waste residue (Z / E=1:7), add 1000mL of ethanol to dilute, add 25g of ferric chloride at the same time, stir and raise the temperature to 80°C, heat and stir for 6 hours, then stop heating, and after the reaction is finished, get The reaction solution is detected by HPLC according to the method of the present invention, Z / E=63 / 37, the reaction solution is purified by the existing separation and purification method, and 265g furan ammonium salt product can be obtained, and the calculated yield is 53%. The product The purity detected by HPLC is ≥99.6%, and the trans-isomer content is ≤0.10%. The product is a white solid, and all indicators fully meet the needs of industrial production.

[0054] Measurement results such as figure 1 and figure 2 as shown, figure 1 is the high performance liquid chromatogram of furan ammonium salt; by figure 1 It can be concluded that:

[0055]

[0056]

[0057] figure 2 It is the NMR spectrum of...

Embodiment 2

[0059] Weigh 500g of furan ammonium salt waste residue liquid (Z / E=1:7), add 1000mL DMF to dilute, add 5% acetic acid at the same time, stir and raise the temperature to 90°C, heat and stir for 6 hours, then stop heating, and the obtained The reaction solution is detected by HPLC according to the present invention, Z / E=59 / 41, and purified by the existing separation and purification method, 257g furan ammonium salt product can be obtained, the calculated yield is 51%, and the purity of the product is detected by HPLC ≥99.5%, and trans isomer content ≤0.10%, the product is a white solid, and the light transmittance and turbidity of the product fully meet the needs of industrial production.

Embodiment 3

[0061] Weigh 500g of furan ammonium salt waste residue (Z / E=1:7), add 1200mL of DMF to dilute, add 25g of ferric chloride at the same time, stir and raise the temperature to 90°C, heat and stir for 8 hours, stop heating, and get The reaction solution is detected by HPLC according to the method of the present invention, Z / E=69 / 31, the reaction solution is purified by existing separation and purification methods, and 260g of furan ammonium salt product can be obtained, and the calculated yield is 52%. The product The purity detected by HPLC is ≥99.6%, and the trans-isomer content is ≤0.10%. The product is a white solid, and all indicators fully meet the needs of industrial production.

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Abstract

The invention provides a method for recycling furan ammonium salt from furan ammonium salt waste liquid. The method comprises the following step: reacting by virtue of furan ammonium salt waste slag liquid in the presence of a solvent and a catalyst, wherein the catalyst is selected from one or more of metal chlorate, metal sulfate, metal nitrate, hydrogen phosphate salt, metal oxide, inorganic acid, organic acid and inorganic base, and metal is selected from one or more of sodium, potassium, calcium, magnesium, aluminum, zinc, iron and cobalt, and the reaction temperature is 50-150 DEG C. According to the method, (Z)-formula furan ammonium salt is directly converted from (E)-formula furan ammonium salt through a one-step method by utilizing the furan ammonium salt waste slag liquid at a specific temperature in a special catalyst system in the presence of the solvent, and finally a thermodynamically stable furan ammonium salt product is obtained. The method includes simple steps and is economic, environmentally friendly and suitable for industrial production, the recycling yield of furan ammonium salt is effectively increased, and meanwhile, the environmental protection pressure of the furan ammonium salt waste liquid is decreased.

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical intermediates, in particular to a method for recovering furan ammonium salt from furan ammonium salt waste liquid. 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. However, in the existing process for preparing cis-furan ammonium salt, due to cis-trans isomerism during oximation in industrial production, organic waste residue liquid of trans-furan ammonium salt isomers will inevitably be produced. This not only seriously wastes chemical raw materials, energy, and human resources, reduces production efficiency and economic benefits, but also poses environmental pollution and safety hazards du...

Claims

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Application Information

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IPC IPC(8): C07D307/54
CPCC07D307/54
Inventor 薛李冰刘长宝韩福社李永生戚福玲刘丽娟王春艳赵立成
Owner 四平市精细化学品有限公司
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