Ethyl Acetate → HCID 178430192, compound

Participants

Reaction Steps

To 7G (140 mg, 0.296 mmol) in THF (2 mL) was added a 1 M THF solution of TBAF (0.400 1 nL, 0.400 mmol). After stirring at rt for 2 h, saturated aqueous ammonium chloride and EtOAc were added and the layers were separated. The organic layer was washed with brine then dried (MgSO4), filtered and concentrated. The resulting residue was purified twice via preparative HPLC (YMC ODS C-1 8, 30×100 mm, eluting with 50-80% solvent B (A=90% H2O-10% MeOH and B=10% H2O-90% MeOH) over 15 min; Flow rate at 40 mL/min; UV detection at 220 nm) to provide the title compound (50.0 mg) as a white foam. MS: m/z 358 [M−H]−.

Provenance & Evidence