反应详情

3-[7-Chloro-5-(2-trifluoromethylphenyl)-1H-benzimidazol-2-yl]-1-oxa-2-aza-spiro[4.5]dec-2-ene (2.39 g, 5.52 mmol) was placed in a 100 mL round-bottom flask. EtOAc (10 mL) was added, and the solid was allowed to dissolve. HCl (5.52 mL, 5.52 mmol, 1 M in ether) was added dropwise via syringe with swirling to ensure sufficient mixing. The mixture was sonicated for 2 min, resulting in a white precipitate, which was isolated by filtration and washed twice with EtOAc (10 mL) then once with ether (20 mL). The solid was dried under high vacuum, yielding the title compound (2.43 g, 94%). 1H-NMR (400 MHz, d6-DMSO) δ: 7.86 (d, J=7.8 Hz, 1H), 7.75 (t, J=7.5 Hz, 1H), 7.65 (t, J=7.6 Hz, 1H), 7.51 (d, J=7.6 Hz, 1H), 7.38 (s, 1H), 7.26 (s, 1H), 3.33 (s, 2H), 1.63-1.81 (m, 6H), 1.32-1.58 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C22H19ClF3N3O: 434.1 (M+H). found: 434.4.

1. dissolutionto dissolve
2. customThe mixture was sonicated for 2 min
3. customresulting in a white precipitate
4. customwhich was isolated by filtration
5. washwashed twice with EtOAc (10 mL)
6. customThe solid was dried under high vacuum