Hydrochloric Acid → 1-[3-(4-Chlorophenyl)-1,2-oxazol-5-yl]methanamine
反応式
[Br-].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]=[C:12]([CH2:14][N+:15]34CN5CN(CN(C5)C3)C4)[O:11][N:10]=2)=[CH:5][CH:4]=1.Cl>CO>[NH2:15][CH2:14][C:12]1[O:11][N:10]=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([Cl:2])=[CH:4][CH:5]=2)[CH:13]=1参加物
4
実験手順
A 205 g. portion of the product of Example 5 was dissolved in 1.5 l. of methanol and 250 ml. of concentrated hydrochloric acid was added. The mixture was stirred at reflux temperature overnight, and the solvent was then evaporated under vacuum. The residue was neutralized with aqueous sodium hydroxide and the product was extracted from the aqueous mixture with methylene dichloride and was purified by evaporating the solvent and recrystallizing the residue from ethanol-petroleum ether. The product was 78 g. of 5-aminomethyl-3-(4-chlorophenyl)isoxazole, m.p. 81°.
後処理
- temperatureat reflux temperature overnight
- customthe solvent was then evaporated under vacuum
- extractionthe product was extracted from the aqueous mixture with methylene dichloride
- customwas purified
- customby evaporating the solvent
- customrecrystallizing the residue from ethanol-petroleum ether
出典と根拠
- ORDレコード
- ord-10fa5e704fcc4497afef9de6594f0517
- 出典データセット
- uspto-grants-1980_05
- 特許番号
- US04203994
反応ノート
読み込み中…