Method for recovering furan ammonium salt from furan ammonium salt waste residue

A technology of furan ammonium salt and waste residue liquid, which is applied in the direction of organic chemistry, can solve the problem of low production cost, and achieve the effects of low production cost, good quality and high product yield

Active Publication Date: 2014-02-05
SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of method that reclaims furan ammonium salt from furan ammonium salt waste slag liquid, makes trans isomer by-product directly convert into cis product, this not only solves the environment

Method used

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  • Method for recovering furan ammonium salt from furan ammonium salt waste residue
  • Method for recovering furan ammonium salt from furan ammonium salt waste residue
  • Method for recovering furan ammonium salt from furan ammonium salt waste residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 500g furan ammonium salt waste residue liquid (E / Z=90:10), diluted with 3000ml water, was added to a 5L photochemical reactor. Utilize 313nm ultraviolet light generated by a high-pressure mercury lamp of 500W to irradiate for 3 hours while stirring, and the temperature in the reactor is controlled at 50°C. The reaction solution obtained after the reaction was detected by HPLC, E / Z=55 / 45. The reaction solution was processed by a known separation method to obtain 195 g of the furan ammonium salt product, and the product yield was 39%.

[0024] The furan ammonium salt product described here refers to the chemical name (Z)-2-methoxyimino-2-(furan-2-yl)ammonium acetate, (alias, methoxyiminofuran ammonium acetate;( Z) ammonium furyl salt; the English name is Syn-2-Methoxyimino-2-(2-Furyl)-Acetic Acid-Ammonia Salt) product.

Embodiment 2-11

[0026] The treatment process of ammonium furan salt waste residue liquid is completely with embodiment 1 among the embodiment 2-11. Embodiment 2-11 was completed by changing the type and amount of diluting solvent used, photochemical reactor light source and wavelength, reaction time, reaction temperature, quality of furan ammonium salt waste residue liquid and other variables. The specific test data are shown in Table 1.

[0027] The test data of table 1 embodiment 2-11

[0028]

[0029]

[0030] The product that embodiment 1-11 obtains is done quality inspection, and result is as follows:

[0031] The product appearance that embodiment 1-11 obtains is all white crystalline powder;

[0032] Identification (HPLC): the products that embodiment 1-11 obtains all meet the requirements;

[0033] Content (HPLC): the products obtained in Examples 1-11 are all ≥ 99.5%;

[0034] Moisture (K.F): the products obtained in Examples 1-11 are all ≤0.20%;

[0035] Absorbance: the p...

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Abstract

The invention belongs to the field of preparation of medical intermediates, and specifically relates to a method for recovering a furan ammonium salt from furan ammonium salt waste residue. The method comprises the following steps: dissolving furan ammonium salt waste residue in a solvent, and then adding into a photochemical reactor to react, wherein the wavelength of a light source of the photochemical reactor is 254-540nm, and a medium pressure mercury lamp or a high pressure mercury lamp is used as the light source in the photochemical reactor. According to the method provided by the invention, trans-form byproducts in the furan ammonium salt waste residue are fully converted into cis-form products by ultraviolet irradiation in appropriate bands through a photo-isomerization principle, thereby realizing effective utilization of waste to the maximum extent. Not only is the pollution reduced, but also the yield of the product is further increased. The cis-form products in the reaction process are not damaged and can be fully recovered in a reaction system, so that the yield of the product is high. The reaction process is simple, no other reaction raw materials are consumed in the reaction process, and the production cost is low.

Description

technical field [0001] The invention belongs to the field of preparation of pharmaceutical intermediates, in particular to a method for recovering furan ammonium salt from furan ammonium salt waste residue liquid. Background technique [0002] Ammonium furan (chemical name: (Z)-2-methoxyimino-2-(furan-2-yl) ammonium acetate) is an important intermediate of the cephalosporin antibiotic cefuroxime, and is used in the preparation of ammonium furan During the process, about 10%-15% of the trans-isomer by-product - (E)-2-methoxyimino-2-(furan-2-yl) acetic acid ammonium is generated, and in the refining process , a small amount of furan ammonium salt product - (Z)-2-methoxyimino-2-(furan-2-yl) ammonium acetate was mixed into the waste residue, forming a brown-black furan ammonium salt waste residue liquid. The generation of this waste residue liquid not only reduces the yield of furan ammonium salt product, but more serious is the environmental protection problem that its existen...

Claims

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Application Information

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IPC IPC(8): C07D307/54
CPCC07D307/54
Inventor 宋道淮蔡会敏解春章张志元王光政张德仕
Owner SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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