Method for removing salt from hydrochloride-1-amido glycolyurea

A technology of aminohydantoin and hydantoin, which is applied in the field of chemical purification, can solve the problems of yellow appearance, affecting drug yield and quality, and achieve the effect of improving drug quality and yield

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 67°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, 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 solid dispersion, keep warm for 55 minutes, after the heat preservation...

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Abstract

The invention provides a desalting method for 1-aminohydantoin hydrochloride in the field of chemical purification. The invention adopts a technical proposal that: acetone is used to treat a crude product of 1-aminohydantoin hydrochloride produced with raw materials of acetone semicarbazone hydantion, methyl sodium and ethyl chloroacetate to produce acetone semicarbazone-1-amino hydantion which is heated for circumfluence in a water solution of hydrochloric acid of which the pH value is equal to 1 to 2 to produce desalted 1-aminohydantoin hydrochloride. The content of sodium chloride in the purified 1-aminohydantoin hydrochloride is below 0.5 percent, so that salt content is lowered significantly, the quality of the sequentially synthesized drug is improved, and the production cost is decreased.

Description

technical field [0001] The invention belongs to the field of chemical purification, in particular to a method for desalting 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] Aiming at the above-mentioned shortcomings, the present invention provides...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/80
Inventor 孙涛张建国
Owner SHANDONG FANGXING SCI & TECH DEV
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