Potassium Carbonate → HCID 10237397, compound

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Reaction Steps

The product of Step 2 (0.670 g, 1.39 mmol) is suspended in 28 mL of methanol, and the solution heated to reflux. Dry K2CO3 (0.386 g, 2.8 mmol) is added, and the mixture is stirred at reflux for 1 h. Upon cooling, the solution is diluted with 2.5% aq. NaHCO3 (20 mL) and the methanol removed by rotary evaporation. The resulting aqueous phase is extracted with EtOAc (5×30 mL), and the combined organic layers are dried (MgSO4). Solvent is evaporated under vacuum, and the crude material purified by silica gel column chromatography (gradient 0–4% MeOH-DCM) to afford the title compound as a white solid. Yiled 0.309 g (58%). Rf=0.13 (5% MeOH-DCM). M.p. 193°–194° C.

Provenance & Evidence