HCID 59315469, compound → HCID 59315022, compound

Participants

Reaction Steps

To Intermediate 8A (10.0 g, 27.0 mmol) in MeOH (250 ml) and EtOAc (150 ml) was added 10% Pd/C (0.5 g, 4.70 mmol) under a stream of nitrogen. The system was purged and degassed 3× with nitrogen, then the hydrogen balloon was introduced. The system was purged and degassed with hydrogen 3×. The mixture was stirred at rt overnight after addition of 0.5 mL of conc. HCl. The catalyst was filtered carefully over CELITE® under a stream of nitrogen and washed with methanol. The filtrate was concentrated and dried to give Intermediate 8B as an off-white solid (9.3 g). MS (ESI) (m/z) 341 [M+H]+; 1H NMR (400 MHz, DMSO-d6) δ ppm 0.85-1.08 (m, 4H) 1.38 (d, J=48.37 Hz, 9H) 2.67-2.78 (m, J=4.40 Hz, 1H) 2.84 (s, 3H) 4.68 (s, 2H) 5.94-6.30 (m, 2H) 6.39 (s, 1H) 7.44 (d, J=8.79 Hz, 1H).

Provenance & Evidence