Water → HCID 19075958, compound

Participants

Reaction Steps

Hydrazine (6.96 g) was added to a suspension of Example 2 (10 g) in ethylene glygol (120 ml) at 38° C. The mixture was heated and potassium carbonate (7.7 g) was added at 65° C. Heating was continued until a temperature of 170° C. was attained. The mixture was cooled to room temperature and poured into a mixture of brine (300 ml), water (300 ml) and ethyl acetate (300 ml). The aqueous layer was extracted with ethyl acetate (2×300 ml) and the combined organic extracts were dried (MgSO4) and concentrated in vacuo. The residue was applied to a silica column and eluted with 30% ethyl acetate in heptane to provide the title compound as an off-white solid (5.1 g).

Provenance & Evidence