ChemicalBook CAS DataBase List 3-Aminoisoxazole

3-Aminoisoxazole synthesis

5synthesis methods

Product Name:3-Aminoisoxazole
CAS Number:1750-42-1
Molecular formula:C3H4N2O
Molecular Weight:84.08

2601-89-0
129 suppliers
$70.00/500 mg

1750-42-1
201 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

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