Water → HCID 135885150, compound

Participants

Reaction Steps

To a solution of Example 18B (205 mg, 0.36 mol) in CH3CN (16 mL) was added H2O (1.1 mL) and molybdenum hexacarbonyl (66 mg, 0.25 mol) and the solution was refluxed for 2 hours. After cooling to room temperature the solvent was removed in vacuo and the crude product was purified by column chromatography on silica gel (3% methanol/chloroform) to give the title compound as a colorless solid (163 mg, 81%): 1H NMR (d6-dmso) δ 14.34 (s, 1H), 9.64 (s, 1H), 8.59 (br s, 2H), 8.13, 8.11 (d, 1H), 7.94 (s, 1H), 7.71-7.49 (m, 4H), 7.27, 7.24 (d, 1H), 2.06-1.96 (m, 1H), 1.91-1.81 (m, 1H), 1.50 (s, 9H), 1.42-1.18 (m, 1H), 1.18-0.94 (m, 1H), 0.75-0.66 (m, 6H), 0.66-0.59 (m, 1H); MS (ESI) m/z 541 (M+H+).

Provenance & Evidence