Trifluoroacetic acid → 3-(Aminomethyl)-N-(3,5-dichlorobenzyl)-N-(4-fluorobenzyl)benzamide
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:32]=[C:33]([Cl:35])[CH:34]=1)[CH2:5][N:6]([CH2:24][C:25]1[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=1)[C:7]([C:9]1[CH:10]=[C:11]([CH:21]=[CH:22][CH:23]=1)[CH2:12][NH:13]C(=O)OC(C)(C)C)=[O:8].C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:13][CH2:12][C:11]1[CH:10]=[C:9]([CH:23]=[CH:22][CH:21]=1)[C:7]([N:6]([CH2:5][C:4]1[CH:32]=[C:33]([Cl:35])[CH:34]=[C:2]([Cl:1])[CH:3]=1)[CH2:24][C:25]1[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=1)=[O:8]参加物
4
実験手順
To a solution of tert-butyl 3-((3,5-dichlorobenzyl)(4-fluorobenzyl)carbamoyl)benzylcarbamate (0.8 g, 1.55 mmol) in CH2Cl2 (8 mL) was added TFA (1.19 mL, 15.5 mmol). The reaction mixture was stirred at rt. for 4 h, concentrated and the residue was diluted with ethyl acetate and saturated aq NaHCO3 solution. The organic layer was separated, washed with brine, dried over MgSO4, and concentrated to give the product as a white solid (0.61 g, 95%). 1H NMR (DMSO-(d6): δ 7.52-7.06 (m, 11H), 4.65-4.40 (m, 4H), 3.72 (s, 2H); MS (ESI): [M+H]+=416.9.