Acetic Acid → HCID 68519399, compound

Participants

Reaction Steps

The crude residue from Step A was dissolved in 5 mL of glacial acetic acid, and the resulting solution was stirred at reflux for 60 h. The cooled solution was concentrated, and the residue was partitioned between 1:1 ethyl acetate:tetrahydrofuran and saturated sodium carbonate aqueous solution. The organic phase was dried over magnesium sulfate, filtered, and concentrated to dryness. Purification of the residue by preparative thin-layer chromatography on silica gel (three successive developments in 95:5, 92.5:7.5, and 90:10 dichloromethane:methanol) afforded the title compound as a stiff foam. LC-MS 406 (M+1).

Provenance & Evidence