Benzyl Bromide → HCID 50987581, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of 3,3-dimethylpiperazin-2-one (prepared according to procedure reported in WO200516900 A1, 6.0 g, 46.8 mmol) in N,N-dimethylformamide (10 ml) was added benzyl bromide (6.68 ml, 56.2 mmol) at 0° C., followed by addition of triethylamine (19.57 ml, 140 mmol). Reaction was stirred for 3 h at 0-25° C. The progress of reaction was monitored by TLC. After completion of reaction, the reaction mixture was diluted with ethyl acetate (100 ml) and water (100 ml). Aqueous layer was extracted with ethyl acetate (50 ml×6). The combined organic phase was washed with brine (50 mL) and dried over sodium sulphate and concentrated under reduced pressure till dryness. Crude compound was adsorbed on 100-200 mesh silica gel and purified by using flash column chromatography method using 5% methanol in dichloromethane as eluent. Title compound was eluted at 5% methanol in dichloromethane (6.2 g, 60.7%).

Provenance & Evidence