Sodium Carbonate → HCID 86699870, compound

Participants

Reaction Conditions

Reaction Steps

A 100-mL three-neck round-bottomed flask equipped with a magnetic stirrer was purged with nitrogen and charged with 122b (560 mg, 2.00 mmol), 103f (830 mg, 2.00 mmol), sodium carbonate (848 mg, 8.00 mmol), dioxane (30 mL) and water (6 mL). This mixture was degassed with nitrogen for 15 min. Tetrakis(triphenyl-phosphine)palladium (231 mg, 0.200 mmol) was added. After heating at 100° C. for 5 h, the reaction mixture was cooled to room temperature and diluted with ethyl acetate (200 mL). The resulting mixture was washed with saturated aqueous sodium bicarbonate (30 mL) and brine (30 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by flash chromatography on silica gel to afford an 81% yield (800 mg) of 122c as a crude product, which was used in next step without further purification.

Provenance & Evidence