Acetic Acid → HCID 67434480, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of Intermediate 89 (11.1 g) in Ethanol (150 mL) was added 2M Aqueous Sodium Hydroxide (36.4 mL). The reaction mixture was then stirred at 80° C. and under nitrogen for 3 h. The reaction mixture was concentrated in vacuo, glacial acetic acid (41.6 mL, 727 mmol) added and allowed to stir at 120° C. and under nitrogen for 2 h. The reaction mixture was concentrated under vacuum. The white solid was suspended and stirred in ether (500 mL) for 5 mins. The white solid was filtered off under vacuum. The solid was suspended in EtOAc (500 mL) and the suspension was refluxed for 45 mins. The white solid was hot filtered under vacuum and washed with EtOAc (100 mL). The filtrate was concentrated under vacuum to give the title compound as a white solid (6.8 g). LC/MS MH+ 439, Rt 1.90 min (5 min run).

Provenance & Evidence