Sodium Hydroxide → HCID 46829880, compound

Participants

Reaction Steps

Intermediate 20 (250 mg) was dissolved in ethanol (10 ml) and the resulting soln was treated with sodium hydroxide, 3M aq (4 ml). The resulting suspension was heated to reflux for 4 h. The reaction mixture was allowed to cool and concentrated in vacuo. The crude residue was taken up in Acetic Acid (10.00 ml) and heated to reflux for 2 h. Reaction mixture concentrated in vacuo and was purified by Reverse Phase chromatography using a 5->80% gradient of Acetonitrile/water with an ammonium carbonate modifier over 12 column volumes. The desired fractions were combined and concentrated under vacuum to give material that was repurified by Reverse Phase chromatography using a 5->80% gradient of acetonitrile water with 0.1% formic acid. The desired fractions were combined and concentrated under vacuum to give the title compound (33 mg). MH+=333 LC/MS MH+333, Rt 1.84 min (5 min run).

Provenance & Evidence