3-Amino-5-methylisoxazole synthesis
- Product Name:3-Amino-5-methylisoxazole
- CAS Number:1072-67-9
- Molecular formula:C4H6N2O
- Molecular Weight:98.1
4368-06-3
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1072-67-9
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$15.00/5 g
Yield:1072-67-9 77%
Reaction Conditions:
Stage #1:3-hydroxybutanenitrile with hydroxylamine hydrochloride;potassium carbonate in water at 20 - 60; for 3 h;
Stage #2: with iron(III) chloride in tolueneReflux;Reagent/catalyst;Temperature;
Steps:
1.2-2.2 The second step:
Combine hydroxylamine hydrochloride (14.0g, 0.20mol), potassium carbonate (70.5g, 0.51mol) and 100mL of water, stir at room temperature for 20 minutes, add compound 2 (14.5g, 0.17mol) obtained in the previous step, heat up to 60°C, and keep for 6 After hours, cool to room temperature, add toluene (200mL) to separate the water layer, add anhydrous ferric chloride (2.76g, 17mmol) to the organic layer, connect to a water separator and heat to reflux to separate water until the amount of separated water reaches the theoretical value, then cool down, Add concentrated hydrochloric acid dropwise to adjust pH=1-2, stir for 1 hour, separate the layers, discard the organic layer, the water layer is dissolved with 30percent sodium hydroxide to adjust pH=11-13, a large amount of precipitation is precipitated, filtered, and dried to obtain a light yellow. The crystalline 3-amino-5-methylisoxazole was 12.8 g, the HPLC purity was 98.8percent, and the yield was 77percent.
References:
Pulasi Science And Technology (Shanghai) Co., Ltd.;Lu Dianyun;Qi Weijun;Xiao Haiwang;Cai Weibing CN107602497, 2020, B Location in patent:Paragraph 0024-0025; 0028; 0029-0030; 0033
91377-59-2
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92087-97-3
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4786-20-3
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1072-67-9
291 suppliers
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