Hydrazine hydrate (1:1) → HCID 11659290, compound

Participants

Reaction Conditions

Reaction Steps

Raney Ni (19.0 g) was added to a 500 mL 3-necked round bottom flask, followed by washing with anhydrous ethanol (30 mL×3) and then ethanol (50 mL) was added. To the suspension was added a solution of compound 4 (16.6 g, 52.0 mmol, 1.0 eq) in ethanol (230 mL). Hydrazine monohydrate (10.4 g 208 mmol, 4.0 eq) was added dropwise at 50° C., followed by heating to 75° C. for 5 min. Upon cooling to room temperature, the catalyst was removed by suction filtration through celite. The filtrate was evaporated to dryness, then co-evaporated with toluene twice and finally dried at 60-65° C. for 30 min under reduced pressure to give compound 1 (14.8 g) in 99% yield.

Provenance & Evidence