Water → HCID 117677449, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of Compound 8 (1.36 g, 2.458 mmol) and ammonium hydroxide (25 ml, 180 mmol) in 1,4-dioxane (25 ml) was heated in a sealed tube at 80° C. for a period of 1 hr. The solution was cooled to room temperature, and water was added. The aqueous layer was extracted twice by dichloromethane and the combined organic extracts were dried (Na2SO4), filtered and concentrated under vacuum. The residue was then purified by column chromatrography on silica gel (EtOAc/hexanes) to give the title compound. 1H NMR (CDCl3) δ 10.65-10.64 (m, 1H), 7.89-7.43 (m, 2H), 7.43-7.39 (m, 1H), 7.30-7.26 (m, 1H), 4.99 (s, 2H), 4.71-4.69 (m, 1H), 4.63-4.58 (m, 2H), 4.08 (s, 3H), 3.90-3.86 (m, 2H), 2.59-2.54 (m, 1H), 2.47-2.46 (m, 1H), 2.17 (s, 1H), 1.84-1.76 (m, 2H), 1.54 (s, 3H), 1.27 (s, 3H); LCMS 2.01 min, 444 (M+H)

Provenance & Evidence