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Method for synthesizing fosfomycin phenylethylamine calt

A technology of left-phosphorus-right-ammonium salt and phenethylamine, applied in the field of synthesis of left-phosphorus-right-ammonium salt, which can solve the problems that restrict product production cost reduction, safety hazards, and high pollution discharge, so as to be beneficial to production organization management and eliminate safety hazards , Ethanol consumption reduction effect

Inactive Publication Date: 2010-06-30
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for synthesizing left phosphorus and right ammonium salts. After hydrogenation, there is no need for distillation and separation of ethanol, and the epoxidation reaction is directly carried out to overcome the high energy consumption and pollution caused by distillation and separation of ethanol in the prior art synthesis method. High, there are potential safety hazards, the production cost of the product is restricted, and the long-term application of ethanol will reduce the catalytic performance of the palladium carbon catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] In the three-necked flask equipped with stirring and a thermometer, add 20ml of the hydrogenation reaction solution that has filtered out the palladium-carbon catalyst, start stirring, add 5.6g of ethanol with a content of 95%, then add a saturated aqueous solution of 0.05g of sodium bicarbonate, Control the temperature at 30-40°C, add 7.6295g of 95% vortex-α-phenylethylamine, continue stirring for 20 minutes, then add 0.318g of sodium tungstate and 0.066g of disodium EDTA in a saturated aqueous solution into the bottle , heat up to 40-50°C, add 7.9055g of hydrogen peroxide with a content of 27.5%, heat up to 50-55°C, keep warm for 1 hour, then cool to -5-10°C, keep warm for 1 hour, crystallization is precipitated, filter, use Wash the filter cake with 10 g of ethanol with a content of 95% to obtain swirl salt, which is then separated and refined to obtain Zuo salt.

Embodiment 2

[0012] In the three-necked flask equipped with stirring and a thermometer, add 20ml of the hydrogenation reaction solution that has filtered out the palladium-carbon catalyst, start stirring, add 5.6g of ethanol with a content of 95%, then add a saturated aqueous solution of 0.05g of sodium bicarbonate, Control the temperature at 30-40°C, add 8.1158g of 95% vortex-α-phenylethylamine, continue stirring for 20 minutes, then add 0.318g of sodium tungstate and 0.066g of disodium EDTA into the bottle. , heat up to 40-50°C, add 7.9055g of hydrogen peroxide with a content of 27.5%, heat up to 50-55°C, keep warm for 1 hour, then cool to -5-10°C, keep warm for 1 hour, crystallization is precipitated, filter, use Wash the filter cake with 10 g of ethanol with a content of 95% to obtain swirl salt, which is then separated and refined to obtain Zuo salt.

Embodiment 3

[0014] In a three-necked flask equipped with stirring and a thermometer, add 20ml of the hydrogenation reaction solution that has filtered out the palladium-carbon catalyst, start stirring, add 5.6g of ethanol with a content of 95%, then add a saturated aqueous solution of 0.124g of sodium bicarbonate, Control the temperature at 30-40°C, add 7.6295g of 95% vortex-α-phenylethylamine, continue stirring for 20 minutes, then add 0.318g of sodium tungstate and 0.066g of disodium EDTA in a saturated aqueous solution into the bottle , heat up to 40-50°C, add 7.9055g of hydrogen peroxide with a content of 27.5%, heat up to 50-55°C, keep warm for 1 hour, then cool to -5-10°C, keep warm for 1 hour, crystallization is precipitated, filter, use Wash the filter cake with 10 g of ethanol with a content of 95% to obtain swirl salt, which is then separated and refined to obtain Zuo salt.

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Abstract

The invention discloses a method for synthesizing fosfomycin phenylethylamine calt. The invention relates to the fine chemical field. The method of the invention comprises the following steps: under the condition of stirring, after the hydrogenation reaction is finished, adding 95% mass-content ethanol into the hydrogenation solution in which palladium-carbon catalyst is filtrated; adding sodium bicarbonate saturated solution while stirring; controlling temperature within the range of 30-40 DEG C, then adding DL-alpha-phenylethylamine or D-alpha-phenylethylamine; stirring continuously and adding the aqueous solution of sodium tungstate and EDTA disodium salt; heating the reaction system to 40-50 DEG C and adding hydrogen peroxide, and then heating again till the temperature reaches 50-55 DEG C and maintaining the temperature; cooling to 5 below-10 below DEG C and maintaining the temperature; and washing filter cake with ethanol after filtration and separation, thus obtaining the levorotary-dextrorotatory mixed salts or the crude levorotary salts. The obtained levorotary-dextrorotatory mixed salts are separated to yield crude levorotary salts, and further the crude levorotary salts are refined to form fine levorotary salts. The method has the advantages of simple process, convenient operation, high safety, low material consumption, less pollution discharge, low cost, and short production cycle.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for synthesizing left phosphorus and right ammonium salts. Background technique [0002] Fosfomycin sodium [(-)-cis-1,2-epoxypropyl phosphate sodium] (hereinafter referred to as fosfomycin sodium) is a new broad-spectrum antibiotic, IR 2S-(-)-cis-1, 2-Epoxypropyl phosphate-R-(+)-α-phenethylamine salt (hereinafter referred to as left phosphorus right amine salt or left salt) is an important intermediate in the chemical synthesis of fosfomycin sodium by Glamkowski method . The main production steps of left phosphorus and right amine salt include: esterification: propynyl alcohol and phosphorus trichloride react in toluene solvent under reduced pressure to generate allenylphosphoryl dichloride and hydrogen chloride, and the generated hydrogen chloride is vacuum belted After the reaction is completed, toluene and excess phosphorus trichloride are distilled and separated to ob...

Claims

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Application Information

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IPC IPC(8): C07F9/38C07C211/27
Inventor 张庆武
Owner NORTHEAST PHARMA GRP
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