반응식
[ClH:1].C(OC([N:9]1[C@H:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C@H:12]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:11]=[C:10]1[NH:26][CH2:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[F:35])=O)(C)(C)C>CCOC(C)=O>[ClH:1].[C:14]1([C@H:13]2[C@@H:12]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[NH:11][C:10]([NH:26][CH2:27][CH2:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[F:35])=[N:9]2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1참가 물질
4
실험 절차
Hydrogen chloride is bubbled into a solution of 91 (0.37 g, 0.81 mmol) in EtOAc (10 mL) for 1 min, and the solution is stirred at RT overnight. The solvent is removed by rotary evaporation, and the residue crystallized from dichloromethane and Et2O to give 0.21 g of the product 92. 1H NMR (DMSO-d6) δ 9.10 (t, 1H), 8.43 (s, 1H), 8.58 (s, 1H), 7.40 (t, 1H), 7.30-7.15 (m, 1H), 7.15-6.90 (m, 8H), 6.80-6.55 (m, 4H), 5.15 (s, 2H), 3.80-3.45 (m, 2H), 3.10-2.85 (m, 2H); MS: m/z 360 (M++1).
후처리
- customThe solvent is removed by rotary evaporation
- customthe residue crystallized from dichloromethane and Et2O
출처 및 근거
- ORD 기록
- ord-94eabe72417e4de19ba079e95c299493
- 출처 데이터셋
- uspto-grants-2008_02
- 특허 번호
- US07326792B2
연결된 노트
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