[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([CH2:14][N:15]3[C:21](=[O:22])[C@@H:20]([NH:23][C:24](=[O:36])[C@@H:25]([N:27](C)[C:28](=O)OC(C)(C)C)[CH3:26])[C@H:19]([CH3:37])[N:18]([C:38](=[O:44])[CH2:39][S:40]([CH3:43])(=[O:42])=[O:41])[C:17]4[CH:45]=[CH:46][CH:47]=[CH:48][C:16]3=4)=[CH:8][C:9](=[O:13])[O:10]2)=[CH:5][CH:4]=1.[C:49]([OH:55])([C:51]([F:54])([F:53])[F:52])=[O:50]>C(Cl)Cl>[F:52][C:51]([F:54])([F:53])[C:49]([OH:55])=[O:50].[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([CH2:14][N:15]3[C:21](=[O:22])[C@@H:20]([NH:23][C:24](=[O:36])[C@@H:25]([NH:27][CH3:28])[CH3:26])[C@H:19]([CH3:37])[N:18]([C:38](=[O:44])[CH2:39][S:40]([CH3:43])(=[O:42])=[O:41])[C:17]4[CH:45]=[CH:46][CH:47]=[CH:48][C:16]3=4)=[CH:8][C:9](=[O:13])[O:10]2)=[CH:5][CH:4]=1To a rt solution of tert-butyl(S)-1-((3S,4S)-1-((7-methoxy-2-oxo-2H-chromen-4-yl)methyl)-4-methyl-5-(2-(methylsulfonyl)acetyl)-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-ylamino)-1-oxopropan-2-yl(methyl)carbamate (42.7 mg, 62.4 μmol) in CH2Cl2 (249 μl) was added TFA (62.4 μl). The reaction was stirred at rt for 1.5 h, then concentrated, taken up in H2O, and lyophilized to provide (S)-N-((3S,4S)-1-((7-methoxy-2-oxo-2H-chromen-4-yl)methyl)-4-methyl-5-(2-(methylsulfonyl)acetyl)-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-yl)-2-(methylamino) propanamide 2,2,2-trifluoroacetate (41.2 mg, 95%) as a white solid. MS m/z 585 (MH)+.
Wird geladen…