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A cooling-dissolution coupled crystallization method for refining left phosphorus and right ammonium salt

A left phosphorus right amine salt and crystallization technology, which is applied in the field of separation and purification of fine chemicals, can solve problems such as low equipment utilization, poor operating environment, and large solvent loss, and achieve low solvent loss, small solvent loss, and high volatility small effect

Active Publication Date: 2019-05-03
HUBEI XUNDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method overcomes the shortcomings of low equipment utilization rate, large solvent loss, poor operating environment and high energy consumption that are common in the prior art, and provides a basis for the industrialization of the crystallization and refining process of left phosphorus and right ammonium salts in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In order to verify the feasibility of the new process of the present invention and whether a higher yield can be achieved, a cooling-dissolution coupling crystallization experiment was carried out with the refined salt of the left phosphorus and right amine salt under the premise of saving the removal of impurities. First, 40.22 grams of left phosphorus right amine salt refined salt (dry basis) is mixed with 121.2 grams of deionized water, the mixed solution is stirred and heated to 75 ℃ to completely dissolve, and then allowed to cool to room temperature naturally, filtered and dried to obtain 26.7 grams of refined left phosphorus Dexamine salt. Add 850 g of acetone to the filtrate obtained in the previous step, stir for 30 minutes, and filter. After the filter cake is dried, 5.44 g of refined left phosphorus and dextroamine salt is obtained. A total of 32.14 g of refined left phosphorus dextroamine salt is obtained. The total yield is 79.9% (dry basis). ). The verific...

Embodiment 2

[0024] Mix 40.22 grams of left-phosphor-right amine salt crude salt (wet base) with 120.63 grams of deionized water, then add 8.11 grams of ethylene glycol, heat the mixed solution to 40 ~ 45 ℃, and then add 5.05 grams of 50% mass fraction Hydrogen peroxide, oxidation reaction for 30min. After the oxidation reaction is completed, the temperature of the mixed solution is increased to 50°C, and 0.6 g of activated carbon is added for decolorization, and heating is continued to raise the temperature of the mixed solution to 70°C, and the activated carbon is suction filtered after the materials are completely dissolved. Wash the activated carbon with an appropriate amount of deionized water, and combine the washing water and the filtrate. The mixed filtrate was naturally cooled to 25-26° C., filtered and dried to obtain 22.92 g of refined left-phosphor-right-amine salt. Add 1000 grams of acetone to the filtrate in the previous step, stir for 30 minutes and then filter. After the fi...

Embodiment 3

[0026] Mix 5.00 grams of left-phosphor-right amine salt crude salt (wet base) with 15.26 grams of deionized water, then add 1.04 grams of ethylene glycol, heat the mixed solution to 40~45°C, and then add 0.69 grams of hydrogen peroxide (50%), Oxidize for 30min. After the oxidation reaction is completed, the temperature of the mixed solution is increased to 50°C, and 0.07 g of activated carbon is added for decolorization, and heating is continued to raise the temperature of the mixed solution to 70°C. After the materials are completely dissolved, the activated carbon is suction filtered out. Wash the activated carbon with an appropriate amount of deionized water, combine the washing water and the filtrate, cool the mixed filtrate to 25-26°C, filter and dry to obtain 2.55 g of refined left-phosphor-right-amine salt. Add 137 grams of acetone to the filtrate in the previous step, stir for 30 minutes and then filter. After drying the filter cake, 0.98 grams of refined left phosphoru...

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Abstract

The invention relates to the technical field of compound separation and purification and in particular relates to a method for refining fosfomycin phenylethylamine salt through cooling-solvating-out coupling crystallization. The method comprises the following steps: with deionized water as a solvent, dissolving crude salt, then adding ethylene glycol, heating the solution to 40-45 DEG C, then oxidizing with hydrogen peroxide and decolorizing with activated carbon, stirring, heating the mixed solution to 70-75 DEG C, filtering the heated solution, cooling filtrate to 20-30 DEG C for crystallization, filtering, adding acetone into filtrate, carrying out solvating-out crystallization, filtering again, distilling filtrate, and then separating acetone and water to be recycled, wherein the yield of fosfomycin phenylethylamine salt refined product obtained after crystallization for twice reaches up to more than 80%. The method provided by the invention is simple in technology and can be carried out at normal temperature, cryogenic crystallization is not needed, energy consumption is low, the solvent, acetone, and water can be basically completely recycled, and fewer pollutants are discharged.

Description

Technical field [0001] The present invention relates to the technical field of separation and purification of fine chemicals, in particular to a method for refining levofos dextroamine salt through cooling-elution coupling crystallization. Background technique [0002] Levophosphoramine salt is also called fosfomycin levorotatory phenethylamine salt, its scientific name is L-cis-1,2-epoxypropylphosphonic acid-D-α-phenethylamine salt, which is the preparation of fosfomycin by the Glamkowski method Intermediates for new chromatographic antibacterial drugs such as sodium, fosfomycin calcium, fosfomycin tromethamine, etc. Industrial refining of left-phosphor-right amine salt is achieved by cooling and crystallization with ethanol as a solvent. Since the solubility of the left phosphorus and right amine salt in ethanol is relatively small, and the whole system is easy to completely solidify at low temperature, the amount of ethanol used to actually dissolve the left phosphorus and ri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/655C07C211/27C07C209/00
CPCC07F9/65505
Inventor 龙秉文谢竞祺王子乐丁一刚查树义杜治平刘生鹏邓伏礼
Owner HUBEI XUNDA PHARMA