Sulfuric Acid → HCID 136383512, compound

Participants

Reaction Steps

To a suspension of the product of Example 74C (1.0 g, 1.8 mmol) in acetonitrile (16 mL) at 0° C. was added conc. H2SO4 (8 mL). The reaction mixture was warmed to room temperature and stirred for 2 h. The solution was poured unto ice (100 g) and extracted with 3:1 dichloromethane:isopropanol (3×50 mL). The organic extracts were combined, dried (Na2SO4), and concentrated in vacuo. The resulting residue was dried under high vacuum to give the title compound as a yellow solid (0.98g, 92%). 1H NMR (300 MHz, DMSO-d6), δ ppm 0.39-0.56 (m, 1H), 0.65 (s, 9H), 0.81-0.98 (m, 1H), 1.77-1.90 (m, 4H), 1.92-2.07 (m, 1H), 6.90-7.04 (m, 2H), 7.39-7.58 (m, 3H), 7.73 (t, J=7.54 Hz, 1H), 8.11 (d, J=7.35 Hz, 1H), 9.16 (s, 1H), 13.38 (s, 1H); MS m/z 497.2 (M+H)+.

Provenance & Evidence