HCID 136396880, compound → HCID 137194559, compound

Participants

Reaction Steps

A solution of Example 53A (40 mg, 0.056 mmol) an in conc. H2SO4 (0.25 mL) was stirred at 25° C. for 1.5 h. The solution was quenched with water, neutralized to pH 7 with 1 N NaHCO3, and extracted with ethyl acetate. The organic extract was concentrated in vacuo. Column chromatography on silica (10% methanol/dichloromethane) afforded the title compound as a yellow solid (23 mg, 75%). 1H NMR (300 MHz, DMSO-d6) δ ppm 0.40-0.59 (m, 1H), 0.64 (dd, J=1.40, 6.62 Hz, 6H), 0.81-0.92 (m, 1H), 0.92-1.03 (m, 1H), 1.18 (t, J=7.17 Hz, 3H), 1.45-1.67 (m, 1H), 1.64-1.82 (m, 1H), 3.11 (s, 3H), 4.12 (q, J=6.99 Hz, 2H), 4.54 (s, 2H), 7.30-7.47 (m, 2H), 7.47-7.87 (m, 4H), 8.06 (d, 1H), 14.92-15.36 (br.s, 1H); MS m/z 621.0 (M+H)+.

Provenance & Evidence