반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([C:14]3[C:15]([CH3:20])=[N:16][O:17][C:18]=3[CH3:19])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][C:3]=1[N+:21]([O-:23])=[O:22].[N:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[C@H:30]([NH2:32])[CH3:31]>CC#N>[CH3:20][C:15]1[C:14]([C:8]2[CH:7]=[C:6]3[C:11]([C:2]([NH:32][C@@H:30]([C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][N:24]=4)[CH3:31])=[C:3]([N+:21]([O-:23])=[O:22])[CH:4]=[N:5]3)=[CH:10][C:9]=2[O:12][CH3:13])=[C:18]([CH3:19])[O:17][N:16]=1참가 물질
4
반응 조건
- 온도
- 60 °C
실험 절차
A mixture of 4-chloro-7-(3,5-dimethyl-4-isoxazolyl)-6-(methoxy)-3-nitroquinoline (for a preparation see Intermediate 18, 0.4 g, 1.2 mmol) and (1R)-1-(2-pyridinyl)ethanamine (2 eq, 0.293 g) in CH3CN (20 ml) was heated at 60° C. for 2 h. The mixture was extracted with DCM. The organic phase washed with saturated aqueous Sodium hydrogen carbonate and dried over Na2SO4. The solvent was evaporated under reduced pressure and the residue taken up in diethyl ether. The precipitate was filtered off and dried in vacuo to give 7-(3,5-dimethyl-4-isoxazolyl)-6-(methoxy)-3-nitro-N-[(1R)-1-(2-pyridinyl)ethyl]-4-quinolinamine (0.4 g) which was used without purification in the next step.
후처리
- extractionThe mixture was extracted with DCM
- washThe organic phase washed with saturated aqueous Sodium hydrogen carbonate
- dry with materialdried over Na2SO4
- customThe solvent was evaporated under reduced pressure
- filtrationThe precipitate was filtered off
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-0804393e07cc4897b024c1a4e2f4f48b
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08557984B2
연결된 노트
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