반응식
[C:1]([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]2[N:23]3[C:18]([CH:19]=[N:20][C:21](O)=[N:22]3)=[CH:17][CH:16]=2)[CH:10]=1)(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH:25]1[C:33]2[C:28](=[CH:29][C:30]([NH2:34])=[CH:31][CH:32]=2)[CH:27]=[N:26]1.CN1C2C(=CC=C(N)C=2)C=N1.CN1C2C(=CC(N)=CC=2)C=N1>>[C:1]([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]2[N:23]3[C:18]([CH:19]=[N:20][C:21]([NH:34][C:30]4[CH:29]=[C:28]5[C:33](=[CH:32][CH:31]=4)[NH:25][N:26]=[CH:27]5)=[N:22]3)=[CH:17][CH:16]=2)[CH:10]=1)(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2]참가 물질
실험 절차
Following the procedure of Example 1311c, N-tert-butyl-3-(2-hydroxy-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-benzenesulfonamide (225 mg, 0.650 mmol) was coupled in parallel fashion with 1H-indazol-5-ylamine (36 mg, 0.27 mmol), [1-methyl-1H-indazol-6-ylamine (43 mg, 0.29 mmol), and 1-methyl-1H-indazol-5-ylamine (41 mg, 0.28 mmol). After evaporation of solvent, residues were purified with ISCO chromatography unit outfitted with a 12 g silica gel column and eluted with a gradient of DCM/MeOH to afford titled products. Yield: 38 mg (13%); LC/MS: 462 (M+H); HPLC: 97% pure, RT=3.11 min; 1H NMR: (DMSO, δ) 12.92 (s, 1H), 9.55 (s, 1H), 9.04 (s, 1H), 8.49 (m, 2H), 8.25 (s, 1H), 8.02 (s, 1H), 7.88 (d, J=8.2, 1H), 7.77 (t, J=8.2, 1H), 7.61 (m, 2H), 7.51 (d, J=8.7, 1H), 7.18 (d, J=4.7, 1H), 6.99 (d, J=4.7, 1H), 1.10 (s, 9H).
후처리
- customAfter evaporation of solvent, residues
- customwere purified with ISCO chromatography unit
- washeluted with a gradient of DCM/MeOH
- customto afford titled products
출처 및 근거
- ORD 기록
- ord-427e439f558244ce977c7acbeda37f4f
- 출처 데이터셋
- uspto-grants-2013_06
- 특허 번호
- US08471005B2
연결된 노트
불러오는 중…