Water → HCID 136383505, compound

Participants

Reaction Steps

To a solution of the product of Example 9 (20 mg, 0.038 mmol) in CH3CN (1.5 mL) was added H2O (100 uL) and molybdenum hexacarbonyl (7 mg, 0.027 mmol) 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 C-1 8 silica gel (70:30:0.1 methanol:H2O:trifluoroacetic acid) to give the title compound as a colorless solid (13 mg, 69%): 1H NMR (d6-DMSO) δ 14.47 (s, 1H), 9.94 (s, 1H), 8.61 (s, 2H), 8.14, 8.11 (d, 1H), 7.70-7.42 (m, 5H), 7.37, 7.34 (d, 1H), 3.01 (s, 3H), 2.03-1.93 (m, 1H), 1.87-1.75 (m, 1H), 1.29-1.14 (m, 1H), 0.96-0.83 (m, 1H), 0.76-0.67 (t, 3H); MS (ESI) m/z 491 (M+H+).

Provenance & Evidence