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Synthesis and purification method of hydrochloride-1-amido glycolyurea

A technology of aminohydantoin and refining method, which is applied in the field of synthesis and refining of 1-aminohydantoin hydrochloride, can solve the problems affecting drug yield and quality, yellow appearance, etc., to improve quality and purity, reduce The effect of production costs

Inactive Publication Date: 2009-06-10
SHANDONG FANGXING SCI & TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The 1-aminohydantoin hydrochloride product prepared by the conventional method contains organic impurities such as acetone aminohydantoin, and the appearance is yellow, and the content is 2% to 3%, which affects the yield and quality of subsequent drug synthesis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Add 40Kg of acetone acetone hydantoin and 180Kg of sodium methoxide into the reaction tank, then close the feed valve, turn on the condenser, steam, stir and raise the temperature to control the temperature in the tank at 65°C, keep warm and reflux for 40 minutes, and make the tank The internal acetone hydantoin was completely dissolved, and 50Kg of methyl chloroacetate was added at the beginning, and after the addition was completed, the reaction was incubated for 30 minutes. Close the steam valve and open the jacket condensate valve to cool down to 40°C. Start to drop 60Kg of hydrochloric acid with a concentration of 30% to PH = 5-6, open the steam valve, raise the temperature to remove water and the methanol produced by reaction, first evaporate to dryness under reduced pressure after normal pressure, open the jacket and cool down the condensed water to below 40°C , add acetone 100Kg, start stirring, heat up to the solid dispersion, keep warm for 50 minutes, after th...

Embodiment 2

[0010] Add 40Kg of acetone acetone hydantoin and 180Kg of sodium methoxide into the reaction tank, then close the feed valve, turn on the condenser, steam, stir and raise the temperature to control the temperature in the tank at 70°C, and keep it under reflux for 45 minutes to make the tank The internal acetone hydantoin was completely dissolved, and 50Kg of methyl chloroacetate was added, and after the addition was completed, the reaction was kept for 40 minutes. Close the steam valve and open the jacket condensate valve to cool down to 50°C. Start to drop 65Kg of hydrochloric acid with a concentration of 30% to PH=5-6, open the steam valve, raise the temperature to remove water and the methanol produced by reaction, evaporate to dryness under reduced pressure at first, open the jacket, and cool down the condensed water to below 40°C , add acetone 100Kg, start stirring, heat up to solid dispersion, keep warm for 60 minutes, after the heat preservation is over, cool down to be...

Embodiment 3

[0012] Add 40Kg of acetone acetone hydantoin and 180Kg of sodium methoxide into the reaction tank, then close the feed valve, turn on the condenser, steam, stir and raise the temperature to control the temperature in the tank at 68°C, and keep it under reflux for 42 minutes to make the tank The internal acetone hydantoin was completely dissolved, and 50Kg of methyl chloroacetate was added, and after the addition was completed, the reaction was incubated for 35 minutes. Close the steam valve and open the jacket condensate valve to cool down to 45°C. Start to drop 63Kg of hydrochloric acid with a concentration of 30% to PH=5-6, open the steam valve, raise the temperature to remove water and the methanol produced by reaction, evaporate to dryness under reduced pressure at first, open the jacket, and cool down the condensed water to below 40°C , add acetone 100Kg, start stirring, heat up to solid dispersion, keep warm for 55 minutes, after the heat preservation is over, cool down ...

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PUM

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Abstract

The invention relates to a method for synthesizing and refining 1-aminohydantoin hydrochloride in the field of chemical synthesis. The method for synthesizing and refining 1-aminohydantoin hydrochloride adopts a technical proposal which comprises the steps of preparation of acetone semicarbazone hydantion, preparation of 1-aminohydantoin hydrochloride, acetone refining, ethanol refining. The method can reduce the content of impurities in the product obtained from 2 to 3 percent to less than 0.5 percent, improve the quality and purity of the product, improve the production quality and purity of subsequent drugs and reduces the production cost.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for synthesizing and refining hydrochloric acid-1-aminohydantoin. Background technique [0002] 1-aminohydantoin hydrochloride is an important intermediate for the synthesis of nitrofurantoin, a therapeutic drug for urinary tract infection. The usual production route of this intermediate is to prepare acetone aminohydantoin from hydrazine hydrate, urea, and acetone, and obtain Acetone aminohydantoin reacts with sodium methoxide, ethyl chloroacetate and hydrochloric acid to obtain hydrochloric acid-1-aminohydantoin. The 1-aminohydantoin hydrochloride product prepared by the conventional method contains organic impurities such as acetone aminohydantoin, which has a yellow appearance and a content of 2% to 3%, which affects the yield and quality of subsequent drug synthesis. Contents of the invention [0003] In order to reduce the impurity content in 1-aminohydantoin h...

Claims

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Application Information

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IPC IPC(8): C07D233/80
Inventor 孙涛仝翔
Owner SHANDONG FANGXING SCI & TECH DEV
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