Methanesulfonic Acid → HCID 58065472, compound

Participants

Reaction Conditions

Reaction Steps

N-(3-Hydroxypropyl)-5-{3-[(1S)-2-methoxy-1-methylethoxy]-5-[4-(methylsulfonyl)phenoxy]phenyl}-1H-pyrrole-2-carboxamide (216 mg, 0.430 mmol) synthesized in Example (37a) was dissolved in tetrahydrofuran (10 mL), and anhydrous methanesulfonic acid (115 mg, 0.660 mmol) and triethylamine (0.18 mL, 1.29 mmol) were added, followed by stirring at room temperature for 4 days, further at 80° C. for 17 hours, under nitrogen atmosphere. A saturated aqueous sodium hydrogencarbonate solution (10 mL) was added, and the solution was separated with ethyl acetate (20 mL). The organic layer was washed with saturated brine, and subsequently dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified using silica gel column chromatography (elution solvent: ethyl acetate/hexane=50%-90%) to afford the desired product (150 mg, yield 72%) as a pale brownish solid.

Provenance & Evidence