CN101450929A - Method for removing salt from hydrochloride-1-amido glycolyurea - Google Patents
Method for removing salt from hydrochloride-1-amido glycolyurea Download PDFInfo
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- CN101450929A CN101450929A CNA2007101147573A CN200710114757A CN101450929A CN 101450929 A CN101450929 A CN 101450929A CN A2007101147573 A CNA2007101147573 A CN A2007101147573A CN 200710114757 A CN200710114757 A CN 200710114757A CN 101450929 A CN101450929 A CN 101450929A
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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
The invention belongs to the chemical purification field, be specially method for removing salt from hydrochloride-1-amido glycolyurea.
Background technology
Hydrochloride-1-amido glycolyurea is the important intermediate of synthetic urinary tract infections medicine furadantin, the common production route of this intermediate is, make the acetone semicarbazone glycolylurea by hydrazine hydrate, urea, acetone, the acetone semicarbazone glycolylurea and sodium methylate, ethyl chloroacetate, the hydrochloric acid reaction that obtain obtain hydrochloride-1-amido glycolyurea.The hydrochloride-1-amido glycolyurea product that ordinary method makes contains organic impuritys such as acetone semicarbazone glycolylurea, the outward appearance jaundice, and content is 2%～3%, influences follow-up medicine synthetic yield and quality.
Summary of the invention
The present invention is directed to the deficiency of above-mentioned existence, a kind of removing salt from hydrochloride-1-amido glycolyurea purification process is provided.The content of sodium-chlor is below 0.5% in the hydrochloride-1-amido glycolyurea behind the purifying, has obviously reduced saltiness, has improved follow-up synthetic drug quality, has reduced production cost.
Technical scheme of the present invention is: will be the hydrochloride-1-amido glycolyurea crude product acetone treatment that raw material makes with acetone semicarbazone glycolylurea and sodium methylate, ethyl chloroacetate, obtain acetone semicarbazone-1-amido glycolyurea, be temperature rising reflux in the aqueous hydrochloric acid of 1-2 with it at PH then, make the hydrochloride-1-amido glycolyurea of desalination.
Detail operations step of the present invention is, acetone semicarbazone glycolylurea 40Kg, the sodium methylate 180Kg that measures added in the retort, close the charging valve then, open condenser, steam, the interior temperature of stirring intensification controlling tank at 65 ℃～70 ℃, insulation refluxed 40～45 minutes, and a jar interior acetone semicarbazone glycolylurea is all dissolved, and began to add methyl chloroacetate 50Kg, finish insulation reaction 30-40 minute.The steam off valve is opened chuck water of condensation valve and is cooled to 40-50 ℃.Begin to drip concentration and be hydrochloric acid 60Kg～65Kg to PH=5-6 of 30%, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is opened the chuck water of condensation and is cooled to below 40 ℃ to doing behind elder generation's normal pressure, adds acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 50-60 minute, insulation finishes, be cooled to below 50 ℃, blowing gets rid of filter, and liquid phase is acetone semicarbazone-1-amido glycolyurea solution, and acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, to PH=1-2 insulation backflow 50-60 minute, the acetone that water and reaction production are deviate from decompression behind the first normal pressure got hydrochloride-1-amido glycolyurea to doing.
The invention has the beneficial effects as follows that the content of sodium-chlor helps the synthetic of follow-up medicine below 0.5% in the hydrochloride-1-amido glycolyurea that obtains, and has improved follow-up drug quality and productive rate.
Embodiment
Embodiment 1
Acetone semicarbazone glycolylurea 40Kg, the sodium methylate 180Kg that measures added in the retort, close the charging valve then, open condenser, steam, the interior temperature of stirring intensification controlling tank at 65 ℃, insulation refluxed 40 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 30 minutes.The steam off valve is opened chuck water of condensation valve and is cooled to 40 ℃.Begin to drip concentration and be 30% hydrochloric acid 60Kg to PH=5-6, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is opened the chuck water of condensation and is cooled to below 40 ℃ to doing behind elder generation's normal pressure, adds acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 50 minutes, insulation finishes, be cooled to below 50 ℃, blowing gets rid of filter, and liquid phase is acetone semicarbazone-1-amido glycolyurea solution, and acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, refluxed 50 minutes to PH=1-2 insulation, decompression is deviate from acetone that water and reaction produce to doing behind the first normal pressure, hydrochloride-1-amido glycolyurea.The content 0.35% of sodium-chlor in the 1-amido glycolyurea that obtains.
Embodiment 2
Acetone semicarbazone glycolylurea 40Kg, the sodium methylate 180Kg that measures added in the retort, close the charging valve then, open condenser, steam, the interior temperature of stirring intensification controlling tank at 70 ℃, insulation refluxed 45 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 40 minutes.The steam off valve is opened chuck water of condensation valve and is cooled to 50 ℃.Begin to drip concentration and be 30% hydrochloric acid 65Kg to PH=5-6, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is opened the chuck water of condensation and is cooled to below 40 ℃ to doing behind elder generation's normal pressure, adds acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 60 minutes, insulation finishes, be cooled to below 50 ℃, blowing gets rid of filter, and liquid phase is acetone semicarbazone-1-amido glycolyurea solution, and acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, refluxed 60 minutes to PH=1-2 insulation, decompression is deviate from acetone that water and reaction produce to doing behind the first normal pressure, hydrochloride-1-amido glycolyurea.The content 0.30% of sodium-chlor in the 1-amido glycolyurea that obtains.
Embodiment 3
Acetone semicarbazone glycolylurea 40Kg, the sodium methylate 180Kg that measures added in the retort, close the charging valve then, open condenser, steam, the interior temperature of stirring intensification controlling tank at 67 ℃, insulation refluxed 42 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 35 minutes.The steam off valve is opened chuck water of condensation valve and is cooled to 45 ℃.Begin to drip concentration and be 30% hydrochloric acid 63Kg to PH=5-6, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is opened the chuck water of condensation and is cooled to below 40 ℃ to doing behind elder generation's normal pressure, adds acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 55 minutes, insulation finishes, be cooled to below 50 ℃, blowing gets rid of filter, and liquid phase is acetone semicarbazone-1-amido glycolyurea solution, and acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, refluxed 55 minutes to PH=1-2 insulation, decompression is deviate from acetone that water and reaction produce to doing behind the first normal pressure, hydrochloride-1-amido glycolyurea.The content 0.25% of sodium-chlor in the 1-amido glycolyurea that obtains.
Claims (5)
1. method for removing salt from hydrochloride-1-amido glycolyurea, it is characterized in that to be the hydrochloride-1-amido glycolyurea crude product acetone treatment that raw material makes with acetone semicarbazone glycolylurea and sodium methylate, ethyl chloroacetate, obtain acetone semicarbazone-1-amido glycolyurea, be temperature rising reflux in the aqueous hydrochloric acid of 1-2 with it at PH then, make the hydrochloride-1-amido glycolyurea of desalination.
2. method for removing salt from hydrochloride-1-amido glycolyurea according to claim 1, the concrete operations step and the condition that it is characterized in that this method are: with the acetone semicarbazone glycolylurea 40Kg that measures, sodium methylate 180Kg adds in the retort, close the charging valve then, drive condenser, steam, stir the interior temperature of intensification controlling tank at 65 ℃～70 ℃, insulation refluxed 40～45 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 30-40 minute, the steam off valve, open chuck water of condensation valve and be cooled to 40-50 ℃, begin to drip concentration and be hydrochloric acid 60Kg～65Kg to PH=5-6 of 30%, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is to doing behind elder generation's normal pressure, opening the chuck water of condensation is cooled to below 40 ℃, add acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 50-60 minute, insulation finishes, and is cooled to below 50 ℃, and blowing gets rid of filter, liquid phase is acetone semicarbazone-1-amido glycolyurea solution, acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, to PH=1-2 insulation backflow 50-60 minute, the acetone that water and reaction production are deviate from decompression behind elder generation's normal pressure gets hydrochloride-1-amido glycolyurea to doing.
3. method for removing salt from hydrochloride-1-amido glycolyurea according to claim 1, the concrete operations step and the condition that it is characterized in that this method are: with the acetone semicarbazone glycolylurea 40Kg that measures, sodium methylate 180Kg adds in the retort, close the charging valve then, drive condenser, steam, stir the interior temperature of intensification controlling tank at 65 ℃, insulation refluxed 40 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 30 minutes, the steam off valve, open chuck water of condensation valve and be cooled to 40 ℃, begin to drip concentration and be 30% hydrochloric acid 60Kg to PH=5-6, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is to doing behind elder generation's normal pressure, opening the chuck water of condensation is cooled to below 40 ℃, add acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 50 minutes, insulation finishes, and is cooled to below 50 ℃, and blowing gets rid of filter, liquid phase is acetone semicarbazone-1-amido glycolyurea solution, acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, to PH=1-2 insulation backflow 50 minutes, the acetone that water and reaction production are deviate from decompression behind elder generation's normal pressure gets hydrochloride-1-amido glycolyurea to doing.
4. method for removing salt from hydrochloride-1-amido glycolyurea according to claim 1, the concrete operations step and the condition that it is characterized in that this method are: with the acetone semicarbazone glycolylurea 40Kg that measures, sodium methylate 180Kg adds in the retort, close the charging valve then, drive condenser, steam, stir the interior temperature of intensification controlling tank at 70 ℃, insulation refluxed 45 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 40 minutes, the steam off valve, open chuck water of condensation valve and be cooled to 50 ℃, begin to drip concentration and be 30% hydrochloric acid 65Kg to PH=5-6, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is to doing behind elder generation's normal pressure, opening the chuck water of condensation is cooled to below 40 ℃, add acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 60 minutes, insulation finishes, and is cooled to below 50 ℃, and blowing gets rid of filter, liquid phase is acetone semicarbazone-1-amido glycolyurea solution, acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, to PH=1-2 insulation backflow 60 minutes, the acetone that water and reaction production are deviate from decompression behind elder generation's normal pressure gets hydrochloride-1-amido glycolyurea to doing.
5. method for removing salt from hydrochloride-1-amido glycolyurea according to claim 1, the concrete operations step and the condition that it is characterized in that this method are: with the acetone semicarbazone glycolylurea 40Kg that measures, sodium methylate 180Kg adds in the retort, close the charging valve then, drive condenser, steam, stir the interior temperature of intensification controlling tank at 67 ℃, insulation refluxed 42 minutes, a jar interior acetone semicarbazone glycolylurea is all dissolved, begin to add methyl chloroacetate 50Kg, finish, insulation reaction 35 minutes, the steam off valve, open chuck water of condensation valve and be cooled to 45 ℃, begin to drip concentration and be 30% hydrochloric acid 63Kg to PH=5-6, open steam valve, water and the methyl alcohol that reacts production heat up, reduction vaporization is to doing behind elder generation's normal pressure, opening the chuck water of condensation is cooled to below 40 ℃, add acetone 100Kg, start stirring, after being warmed up to solid dispersed, be incubated 55 minutes, insulation finishes, and is cooled to below 50 ℃, and blowing gets rid of filter, liquid phase is acetone semicarbazone-1-amido glycolyurea solution, acetone semicarbazone-1-amido glycolyurea is dropped into another retort, add hydrochloric acid 50Kg, to PH=1-2 insulation backflow 55 minutes, the acetone that water and reaction production are deviate from decompression behind elder generation's normal pressure gets hydrochloride-1-amido glycolyurea to doing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101147573A CN101450929A (en) | 2007-11-30 | 2007-11-30 | Method for removing salt from hydrochloride-1-amido glycolyurea |
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| CNA2007101147573A CN101450929A (en) | 2007-11-30 | 2007-11-30 | Method for removing salt from hydrochloride-1-amido glycolyurea |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444045A (en) * | 2021-07-08 | 2021-09-28 | 江西汇和化工有限公司 | Method for purifying cis-hydantoin |
| CN115124518A (en) * | 2022-06-28 | 2022-09-30 | 北京云鹏鹏程医药科技有限公司 | Preparation method of nitrofurantoin with low nitrofural content |
-
2007
- 2007-11-30 CN CNA2007101147573A patent/CN101450929A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444045A (en) * | 2021-07-08 | 2021-09-28 | 江西汇和化工有限公司 | Method for purifying cis-hydantoin |
| CN115124518A (en) * | 2022-06-28 | 2022-09-30 | 北京云鹏鹏程医药科技有限公司 | Preparation method of nitrofurantoin with low nitrofural content |
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Open date: 20090610 |