3-Aminoisoxazole synthesis
- Product Name:3-Aminoisoxazole
- CAS Number:1750-42-1
- Molecular formula:C3H4N2O
- Molecular Weight:84.08
2601-89-0
134 suppliers
$70.00/500 mg
1750-42-1
216 suppliers
$10.00/1g
Yield:1750-42-1 87.8%
Reaction Conditions:
with N-hydroxyurea;sodium hydroxide in N,N-dimethyl-formamide at 10 - 25; for 6 h;Temperature;
Steps:
1-3
Preparation of 3-aminoisoxazole: Put 6.0 kg of liquid caustic soda with a mass concentration of 20% into a 20L reactor, and start stirring;Then put 760g of hydroxyurea and 57g of N,N-dimethylformamide in sequence, and cool down;Below 15°C, start dropping 1.27kg of 2,3-dichloropropionitrile;During the dropping process, keep the temperature at 10-20°C, and the dropping time is about 2 hours.After the addition is complete, keep the temperature at 25±3°C and stir for 4 hours.After the reaction is completed, carbon dioxide is introduced, pH is adjusted to 8-9, and salt is removed by suction filtration.The mother liquor was extracted 3 times with methyl isobutyl ketone, with an amount of 2L each time, and the combined extracts were dried with anhydrous sodium sulfate.Then use 120 g of activated carbon to decolorize, filter, and desolvate the filtrate to obtain 755 g of light yellow oil.The oily substance is then distilled under reduced pressure by an oil pump (high vacuum below 50Pa) to obtain 738g of colorless oily substance, The yield is 87.8%, and the purity is 98.5%.
References:
Yangzhou Tianhe Pharmaceutical Co., Ltd.;Zhang Laiping;Zhao Yunde;Zhu Linfei;Xue Chen;Jin Lei CN112047897, 2020, A Location in patent:Paragraph 0038; 0041-0043; 0045-0047; 0049-0051; 0053-0054
288-14-2
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1750-42-1
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4554-16-9
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1750-42-1
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7341-96-0
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$19.00/250mg
1750-42-1
216 suppliers
$10.00/1g