HCID 118098738, compound → HCID 118098737, compound

Participants

Reaction Steps

17I (0.227 g, 0.272 mmol) was dissolved in methanol (10 mL), degassed (3× Ar/vacuum). Then, Pd—C (0.029 g, 0.027 mmol) was added, and the reaction mixture was degassed again (3× Ar/vacuum). The resulting suspension was stirred under hydrogen (1 atm, balloon) for 1 h. The reaction mixture was filtered though a membrane filter, washed with MeOH (2×2 mL). MeOH was removed under reduced pressure to give 17J (0.199 g, 0.268 mmol, 98% yield) as a yellowish glass, which was lyophilized to give as a yellow solid. MS (ESI) m/z: 744.3 [M+1]+. 1H NMR: (400 MHz, CD3OD) δ ppm 8.04 (1H, d, J=5.77 Hz), 7.58-7.69 (2H, m), 7.50 (1H, d, J=6.02 Hz), 7.43 (1H, d, J=7.78 Hz), 7.24-7.30 (2H, m), 6.86 (1H, d, J=2.01 Hz), 6.50 (1H, dd, J=11.29, 2.01 Hz), 5.71 (1H, s), 5.56 (1H, br. s.), 5.36 (1H, d, J=17.32 Hz), 4.67 (1H, t, J=10.92 Hz), 3.86-3.99 (2H, m), 3.65 (2H, s), 3.41-3.55 (1H, m), 3.28 (3H, br. s.), 2.34 (3H, s), 1.23-1.36 (21H, m).

Provenance & Evidence