Trifluoroacetic acid → HCID 57634625, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of 1-(3-cyanobenzyl)-4-Boc-2-piperazinone (2.5 g, 7.9 mmol) in CH2Cl2 (20 mL) at 0° C. was added TFA (10 mL). The mixture was stirred at 0° C. for 2 h, then the solvents were removed in vacuo. The crude 1-(3-cyanobenzyl)-2-piperazinone TFA salt was partitioned between EtOAc (30 mL) and saturated aqueous sodium bicarbonate solution (30 mL). To the stirred two-phase mixture was added acetic anhydride (1.5 mL, 15 mmol) dropwise over a period of 5 min. The mixture was stirred at ambient temperature for 16 h. The EtOAc layer was separated, dried (MgSO4), filtered, and the solvent was removed in vacuo. The residue was purified on a silica gel column using a gradient mobile phase of 2%, 3%, 4% MeOH in CH2Cl2. 1-(3-cyanobenzyl)-4-acetyl-2-piperazinone was obtained as a solid.

Provenance & Evidence