Tetrahydrofuran → HCID 24996234, compound

Participants

Reaction Conditions

Reaction Steps

To the product of Step B (13.15 g, 35 mmol) in THF (160 mL) was added MeMgBr (1.4 M in toluene/THF, 26.25 mL, 36.75 mmol). After stirring 3 min, 2-methylprop-1-enylmagnesium bromide (0.5 M in THF, 100 mL, 50 mmol) was added and the temperature was increased to 50° C. After 20 min the reaction was cooled, quenched with 2 M HCl and diluted with EtOAc. The reaction was stirred for 3 days before work up. The solution was washed twice with brine, followed by twice with saturated aq NaHCO3. The concentrated residue was purified by flash chromatography on silica gel gradient eluted with 0-25% EtOAc in hexane to afford the title compound. (LC-2) HPLC/MS: 432.2 (M+1), 434.2 (M+3); Rt=4.15 mm.

Provenance & Evidence