Acetic Anhydride → HCID 86744037, compound

Participants

Reaction Steps

A solution of the product of Example 2 (2.9 g), hydroxylamine hydrochloride (0.51 g) and sodium acetate (0.76 g) in acetic acid (30 ml) was stirred for 2 h at room temperature, then acetic anhydride (2.2 g) was added to the reaction. The mixture was heated to 95°-100° for 5 h and then extracted with ethyl acetate. The organic phase was washed with 5% sodium hydroxide and brine, dried over Na2SO4 and evaporated. The residue was purified by column chromatography on silica gel eluting with cyclohexane/ethyl acetate 7:3 to give the title compound (0.45 g) as a yellow solid. M.p. 146°-147°.

Provenance & Evidence