Trifluoroacetic acid → Trifluoroacetic acid

Reaktionsgleichung

C(OC([N:8]1[CH2:17][CH2:16][C:15]2[N:14]=[CH:13][C:12]([NH:18][C:19]3[N:28]=[C:27]4[C:22]([C:23](=[O:40])[N:24]([C:32]5[C:37]([F:38])=[CH:36][CH:35]=[CH:34][C:33]=5[Cl:39])[C:25]5[N:26]4[CH:29]=[CH:30][N:31]=5)=[CH:21][N:20]=3)=[CH:11][C:10]=2[CH2:9]1)=O)(C)(C)C.[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44]>C(Cl)Cl>[Cl:39][C:33]1[CH:34]=[CH:35][CH:36]=[C:37]([F:38])[C:32]=1[N:24]1[C:23](=[O:40])[C:22]2[CH:21]=[N:20][C:19]([NH:18][C:12]3[CH:13]=[N:14][C:15]4[CH2:16][CH2:17][NH:8][CH2:9][C:10]=4[CH:11]=3)=[N:28][C:27]=2[N:26]2[CH:29]=[CH:30][N:31]=[C:25]12.[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44]

Komponenten

Versuchsvorschrift

A mixture of Example 277A (54.6 mg, 0.097 mmol) and trifluoroacetic acid (0.075 mL, 0.970 mmol) in CH2Cl2 (3 mL) was stirred overnight. The solids were filtered, rinsed with CH2Cl2, and dried to provide the title compound as a trifluoroacetic acid salt. 1H NMR (400 MHz, CD3OD) δ 3.29-3.26 (m, 2H), 3.68 (t, J=6.4 Hz, 2H), 4.55 (s, 2H), 7.11 (d, J=1.9 Hz, 1H), 7.44-7.35 (m, 1H), 7.56-7.53 (m, 1H), 7.66-7.60 (m, 1H), 7.91 (d, J=1.9 Hz, 1H), 8.38 (bs, 1H), 8.93 (bs, 1H), 9.26 (s, 1H). MS (ESI+) m/z 463.2 (M+H)+.