Pyridine → HCID 56963344, 화합물
반응식
NC[CH2:3][N:4]([S:28]([CH3:31])(=[O:30])=[O:29])[C:5]1[C:6]([CH:25]2[CH2:27][CH2:26]2)=[CH:7][C:8]2[C:12]([CH:13]=1)=[N:11][N:10]([C:14]1[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][CH:15]=1)[C:9]=2[C:21]([NH:23][CH3:24])=[O:22].[C@@H:32]1([C:40]([OH:42])=[O:41])[CH2:36][CH2:35][CH2:34][C@@H:33]1[C:37]([OH:39])=O.[N:43]1C=CC=[CH:45][CH:44]=1>>[Br:20][C:17]1[CH:18]=[CH:19][C:14]([N:10]2[C:9]([C:21](=[O:22])[NH:23][CH3:24])=[C:8]3[C:12]([CH:13]=[C:5]([N:4]([S:28]([CH3:31])(=[O:30])=[O:29])[CH2:3][CH2:45][CH2:44][NH:43][C:37]([C@H:33]4[CH2:34][CH2:35][CH2:36][C@H:32]4[C:40]([OH:42])=[O:41])=[O:39])[C:6]([CH:25]4[CH2:27][CH2:26]4)=[CH:7]3)=[N:11]2)=[CH:15][CH:16]=1참가 물질
실험 절차
A mixture of Compound (7) (6.4 mg, 0.012 mmol) and cis-1,2-cyclopentanedicarboxylic acid (1.9 mg, 0.014 mmol) in pyridine (0.2 mL) was stirred at RT over the weekend. The solvent was removed under pressure. The crude material was purified by preparative LCMS (5-100% ACN in 0.1% aqueous formic acid) to afford Compound (63) as a white solid (0.7 mg, 8%). ESI-MS m/z calculated for [M+H]+: 660.2/662.2; found: 660.0/662.0; 1H NMR (400 MHz, CDCl3) δ 7.93 (s, 0.5H), 7.87 (s, 0.5H), 7.71 (d, J=8.7 Hz, 2H), 7.51 (dd, J=8.8, 2.2 Hz, 2H), 7.40 (d, J=3.7 Hz, 1H), 6.02-5.92 (m, 1H), 5.87 (d, J=4.1 Hz, 1H), 4.05-3.68 (m, 2H), 3.68-3.40 (m, 1H), 3.35-2.95 (m, 3H), 3.21 (s, 3H), 3.05 (d, J=4.9 Hz, 3H), 2.55-2.37 (m, 1H), 2.28-2.11 (m, 1H), 2.10-1.89 (m, 7H), 1.20-0.90 (m, 3H), 0.72-0.47 (m, 1H).
후처리
- customThe solvent was removed under pressure
- customThe crude material was purified by preparative LCMS (5-100% ACN in 0.1% aqueous formic acid)
출처 및 근거
- ORD 기록
- ord-195478ae02bf4948aecfdd4c476573a3
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08546389B2
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