反应详情

A solution of tert-butyl[2-(3-methoxycarbonyl-benzylsulfanyl)-benzoimidazol-1-yl]-acetate (Precursor H-01b, 31 mg, 0.075 mmol) in TFA/dichloromethane (1:1, 2 ml) is stirred at rt for 4 h. The solvents are removed under a stream of air. The solid residue is suspended in Et2O (2 ml) and sonicated. Filtration, rinsing with Et2O and drying under high vacuum, yields the title compound (19.6 mg) in 73% as a white solid: tR=5.52 min (LC-1), ESI-MS (pos.): m/z 357.25 [M+H]+, ESI-MS (neg.): m/z 355.29 [M−H]+; 1H-NMR (DMSO-d6): δ (ppm) 3.83 (s, 3H, OMe), 4.65 (s, 2H, SCH2), 4.92 (s, 1H, CH2CO2), 7.15-7.21 (m, 2Harom), 7.42-7.48 (m, 2Harom), 7.57 (m, 1Harom), 7.72 (d, 1Harom), 7.81 (d, 1Harom), 8.05 (s, 1Harom).

1. customThe solvents are removed under a stream of air
2. customsonicated
3. filtrationFiltration
4. washrinsing with Et2O
5. customdrying under high vacuum