Hydrochloric Acid → HCID 68731126, compound

Participants

Reaction Steps

To a solution of 3b (30 mg, 0.0632 mmol) in MeOH (1 ml) was added 3N HCl in AcOEt (0.5 ml) under ice cooling, and the mixture was stirred at room temperature for 1 h. A solution of NaHCO3 (139 mg) in H2O was poured into the reaction mixture under ice cooling, and the whole was extracted with AcOEt. The organic layer was washed with brine, dried over Na2SO4, and then concentrated. The residue was crystallized with Et2O to give 8 (67%). 8: colorless powder; 1H-NMR (CD3OD) δ 1.53 (3H, dd, J=1.4, 6.8 Hz), 2.35 (6H, s), 2.77 (2H, t, J=5.4 Hz), 4.06 (2H, t, J=5.4 Hz), 4.64 (1H, brt), 5.53 (2H, dq, J=1.5, 6.8 Hz), 6.74 (2H, d, J=8.6 Hz), 6.85 (2H, d, J=9.2 Hz), 7.18-7.22 (5H, m), 7.27-7.32 (4H, m). HRMS calcd for C27H31N2O3 [M+H]+: 431.2335. Found: 431.2348.

Provenance & Evidence