Hydrochloric Acid → 1-[3-(4-Chlorophenyl)-1,2-oxazol-5-yl]methanamine
반응식
[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]=1참가 물질
4
실험 절차
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°.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-10fa5e704fcc4497afef9de6594f0517
- 출처 데이터셋
- uspto-grants-1980_05
- 특허 번호
- US04203994
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