Trifluoroacetic acid → Trifluoroacetic acid

Participants

Reaction Steps

A solution of 4-((4-methoxybenzyl)((1-methyl-1H-1,2,3-triazol-4-yl)methyl)amino)-6-(((1S,2S)-2-(5-methoxypyridin-2-yl)cyclopropyl)methoxy)-2-methylpyridazin-3(2H)-one (55 mg, 0.11 mmol) in TFA (2 mL) was stirred at room temperature for 2 h, then pH was adjusted to 7˜8 with saturated NaHCO3 solution. Extracted with EtOAc (20 mL*3), washed with H2O and brine, and concentrated. The residue was purified by Prep-HPLC (CH3CN in 0.05% TFA/H2O 30-95% v/v as mobile phase) to give title compound as a TFA salt, the structure was confirmed by NOE. ESI-MS: 398.2 (M+H)+. 1H NMR (400 MHz, MeOD) δ 8.34 (d, 1H), 8.03 (dd, 1H), 7.86 (s, 1H), 7.80 (d, 1H), 5.88 (s, 1H), 4.47 (s, 2H), 4.30 (dd, 1H), 4.11 (dd, 1H), 4.06 (s, 3H), 4.01 (s, 3H), 3.62 (s, 3H), 2.36-2.32 (m, 1H), 2.01-1.96 (m, 1H), 1.41-1.41 (m, 2H).

Provenance & Evidence