Sodium Bicarbonate → HCID 86663418, compound

Participants

Reaction Steps

Sodium hydrogencarbonate (7.15 g, 85.11 mmol) was added to a solution of the crude product (32.1 g) obtained in Example 1h and the compound (37.6 g, 70.9 mmol) obtained in Example 1d in acetonitrile (160 mL) with stirring at room temperature, and the mixture was stirred at reflux temperature under a nitrogen atmosphere for 14 hours. The reaction mixture was left to stand for cooling to room temperature, and then the organic solvent was evaporated under reduced pressure. An aqueous sodium hydrogencarbonate solution was added to the resulting residue, and the mixture was extracted with ethyl acetate. The organic layers were combined and dried with anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=2:1→0:1, v/v) to give the title compound (47.8 g; yield, 93%) as a white solid.

Provenance & Evidence