Hydrochloric Acid → HCID 178478960, compound

Participants

Reaction Steps

3-[7-Trifluoromethyl-5-(2-trifluoromethyl-phenyl)-1H-benzimidazol-2-yl]-1-oxa-2-aza-spiro[4.5]dec-2-ene (524 mg, 1.12 mmol, as prepared in the previous step) was placed in an 8 mL vial, dry MeOH (2 mL) was added, and the mixture was warmed until the solid dissolved. This mixture was added to a mL vial containing ether (20 mL) and 1 M HCl in ether (1.12 mL, 1.12 mmol), resulting in a homogeneous solution. The solution was transferred to a 100 mL round-bottom flask, the solvent was removed under reduced pressure, and the solid was dried under vacuum, giving 469 mg (83%) of the desired HCl salt. 1H-NMR (400 MHz, d6-DMSO) δ: 7.89 (d, J=7.6 Hz, 1H), 7.73-7.81 (m, 1H), 7.71 (s, 1H), 7.63-7.70 (m, 1H), 7.55 (d, J=7.3 Hz, 1H), 7.48 (s, 1H), 3.33 (s, 2H), 1.62-1.83 (m, 6H), 1.33-1.59 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C23H19F6N3O: 468.1 (M+H). found: 468.3. Elemental Analysis Calcd. for C23H19F6N3O: C, 59.10; H, 4.10; F, 24.39; N, 8.99. Found C, 59.06; H, 4.04; F, 24.30; N, 9.04 (% H2O 0.39, Pd <1 ppm).

Provenance & Evidence