OXONIC ACID POTASSIUM SALT synthesis
- Product Name:OXONIC ACID POTASSIUM SALT
- CAS Number:2207-75-2
- Molecular formula:C4H2KN3O4
- Molecular Weight:195.17
64-19-7
97-59-6
2207-75-2
The general procedure for synthesizing potassium oxonate from glacial acetic acid and allantoin was as follows: 3.2 kg of potassium hydroxide was dissolved in 11.4 L of water, added to a 20 L reactor to dissolve, and then cooled to 0~5 °C. 46 g of potassium iodide was added, and 0.9 kg of allantoin was added in batches and stirred until completely dissolved, keeping the temperature at 0~5 °C. Subsequently, 1.8 kg of bromine was slowly added dropwise, and the dropwise time was controlled at 9 hours (the experiment was divided into the first 1-8 groups according to the difference of bromine dropwise time). After the dropwise addition was completed, stirring was continued at 0~5°C for 1 h. Then the temperature was increased to 20~25°C and the reaction was kept at this temperature for 20 h. The reaction was carried out by HPLC. After confirming that the allantoin content was less than 0.6% by HPLC, the reaction solution was cooled to 0~5°C. The pH was adjusted to 5 with acetic acid and the reaction solution was filtered. The filter cake was washed with 3 L of water at 0~5°C and then with 1 L of room temperature ethanol. Finally, potassium oxonate was allowed to precipitate from a white potassium oxide crystalline solid at room temperature.
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Yield:2207-75-2 76.1%
Reaction Conditions:
Stage #1:Allantoin with bromine;potassium iodide;potassium hydroxide in water at 0 - 25; for 30 h;
Stage #2:acetic acid in water; pH=5 at 0 - 5;Time;
Steps:
1 Example 1
3.2Kg potassium hydroxide dissolved in 11.4L water, dissolved after adding 20L reactor,Cooling to 0 ~ 5 ,Add 46g potassium iodide, add 0.9kg allantoin in batches,Stirring dissolved,Temperature control 0 ~ 5 drop 1.8kg bromine to be 9h (according to the different bromine drop time, respectively, as the first 1-8 groups)After completion of the dropwise addition, stirring at 0 to 5 ° C for 1 hour and raising the temperature to 20 to 25 ° C for 20 h,HPLC to detect allantoin less than 0.6%, cooling to 0 ~ 5 , dropping acetic acid to adjust the pH to 5, filtration, 3L0 ~ 5 water washing, 1L room temperature ethanol wash,Dry at room temperature with white oxonate potassium crystalline solid.
References:
Shandong Chuancheng Pharmaceutical Co., Ltd.;Ma, Juliang;Guo, Ming;Liu, Huaizhen CN106083750, 2016, A Location in patent:Paragraph 0019; 0020; 0021
97-59-6
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$6.00/5g
2207-75-2
355 suppliers
$6.00/250mg
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2207-75-2
355 suppliers
$6.00/250mg