Dichloromethane methanol → HCID 87173151, compound

Participants

Reaction Steps

The title compound of Example 3 (600 mg, 1.14 mmol) and Cu(OAc)2 (1.05 g, 5.76 mmol) were dissolved in CH3CN (7.6 mL). This was refluxed for 20 mins. By TLC (10% MeOH/CH2Cl2), starting material was still present, so the mixture was refluxed for an additional 20 mins. By TLC, starting material had been consumed. Removed CH3CN via rotary evaporation and vacuum pump. Residue was then partitioned between ethyl acetate and water. Aqueous phase was discarded and organic phase was washed with brine and dried over Na2SO4. Oily residue was purified via flash column chromatography (a gradient of 100% ethyl acetate to 5% MeOH/CH2Cl2 to 10% MeOH/CH2Cl2) to afford the title compound as a white solid. 1H NMR (CD3OH): consistent with proposed structure. MS (m/z): 1047.3.

Provenance & Evidence