Trifluoroacetic acid → HCID 178436496, 화합물
반응식
[Cl:1][C:2]1[N:3]=[CH:4][N:5](COCC[Si](C)(C)C)[C:6]=1[C:7]([NH:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([O:18][C:19]2[CH:24]=[C:23]([C:25]#[CH:26])[CH:22]=[C:21]([Cl:27])[CH:20]=2)[C:12]=1[F:28])=[O:8].C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:1][C:2]1[N:3]=[CH:4][NH:5][C:6]=1[C:7]([NH:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([O:18][C:19]2[CH:24]=[C:23]([C:25]#[CH:26])[CH:22]=[C:21]([Cl:27])[CH:20]=2)[C:12]=1[F:28])=[O:8]참가 물질
4
실험 절차
To a solution of 4-chloro-N-({4-chloro-3-[(3-chloro-5-ethynylphenyl)oxy]-2-fluorophenyl}methyl)-1-({[2-(trimethylsilyl)ethyl]oxy}methyl)-1H-imidazole-5-carboxamide (98.0 mg, 0.172 mmol) in DCM (5 ml) was added TFA (2.0 ml) and the reaction mixture was stirred at rt for 3 hours. The reaction was quenched with saturated sodium bicarbonate, diluted with EtOAc, and the organic layer was separated. The solvent was removed and the crude material was purified via silica gel chromatography to give 4-chloro-N-({4-chloro-3-[(3-chloro-5-ethynylphenyl)oxy]-2-fluorophenyl}methyl)-1H-imidazole-5-carboxamide (50.0 mg, 0.114 mmol, 66% yield) 1H NMR (400 MHz, DMSO-d6) δ ppm 8.09-8.30 (m, 1H), 7.73 (s, 1H), 7.45 (d, 1H), 7.22-7.36 (m, 2H), 7.08 (s, 1H), 6.88 (s, 1H), 4.49 (d, 2H), 4.37 (s, 1H). LC-MS (ES+) m/z 438.01, [M+H].