Methanol → HCID 16731515, compound

Participants

Reaction Steps

Compound 87A (64 mg, 0.15 mmol) was dissolved in 1.5 mL of THF, treated with 1N KOH in anhydrous methanol (0.32 mL, 0.32 mmol) at rt for 2 h. Diluted the reaction mixture with 30 mL EtOAc, washed with saturated aqueous NaHCO3 solution (10 mL), brine (10 mL×2), dried over MgSO4, filtered and concentrated. The resulting mixture was purified by reverse phase HPLC (Phenomenex Luna 30×250 mm S5 C18, 30 min. gradient time, 25 mL/min, 30-100% B solvent, A=10% MeOH/water, B=90% MeOH/Water), provided the title compound (43 mg). Analytical HPLC retention time 2.947 min (purity 98%). Condition: YMC Combiscreen ODS-A C18 4.6×50 mm column, 4 min gradient, 4 mL/min flow, 0-100% B solvent, A=10% MeOH/water+0.1% H3PO4, B=90% MeOH/Water+0.1% H3PO4. MS (ES) m/z 320.24 [M+H]+, HRMS calcd for [M+H] 320.1166, found 320.1152.

Provenance & Evidence