반응식
[CH3:1][C:2]1[C:6]([C:7]2[CH:12]=[C:11]([N+:13]([O-])=O)[CH:10]=[CH:9][C:8]=2[O:16][CH3:17])=[C:5]([CH3:18])[O:4][N:3]=1>C(OCC)(=O)C>[CH3:1][C:2]1[C:6]([C:7]2[CH:12]=[C:11]([CH:10]=[CH:9][C:8]=2[O:16][CH3:17])[NH2:13])=[C:5]([CH3:18])[O:4][N:3]=1.[CH3:1][C:2]1[C:6]([C:7]2[CH:12]=[C:11]([NH2:13])[CH:10]=[CH:9][C:8]=2[O:16][CH3:17])=[C:5]([CH3:18])[O:4][N:3]=1참가 물질
실험 절차
3,5-Dimethyl-4-[2-(methyloxy)-5-nitrophenyl]isoxazole (for a preparation see Intermediate 61, 68 g, 274 mmol) was dissolved in ethyl acetate (1 l) and the solution washed with sodium sulphite solution (5%, 500 ml). The organic layer was dried (sodium sulphate) and filtered through a 3 cm pad of silica gel. The filtrate was diluted with ethanol (1 l) and added to Pd/C (E101 type NO/W, 10 g) in a 5 l nitrogen/vacuum purged hydrogenation flask under vacuum, The mixture was stirred for 24 h. The mixture was purged with vacuum/nitrogen cycles (×3), filtered through Celite under nitrogen and the filtrate evaporated in vacuo to give [3-(3,5-dimethyl-4-isoxazolyl)-4-(methyloxy)phenyl]amine 3-(3,5-dimethyl-4-isoxazolyl)-4-(methyloxy)aniline (62.3 g).
후처리
- washthe solution washed with sodium sulphite solution (5%, 500 ml)
- dry with materialThe organic layer was dried (sodium sulphate)
- filtrationfiltered through a 3 cm pad of silica gel
- additionThe filtrate was diluted with ethanol (1 l)
- additionadded to Pd/C (E101 type NO/W, 10 g) in a 5 l nitrogen/vacuum
- custompurged hydrogenation flask under vacuum
- customThe mixture was purged with vacuum/nitrogen cycles (×3)
- filtrationfiltered through Celite under nitrogen
- customthe filtrate evaporated in vacuo
출처 및 근거
- ORD 기록
- ord-ef34c290b3404c5c96cb7ef0fe0f8fad
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08557984B2
연결된 노트
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