反应详情

To a solution of 4-acetyl-3-phenyl-piperazine-1-carboxylic acid tert-butyl ester (250 mg, 0.82 mmol) in THF (3 mL) at 0° C. was added 50% TFA/dichloromethane (1 mL). After stirred for 2 h, the reaction mixture was concentrated in vacuo. The residue was diluted with dichloromethane and silica-bound carbonate (2 g, 0.77 mmol/g, Silicycle, Inc.) was added. The reaction mixture was stirred overnight, filtered, and concentrated in vacuo. The residue was purified by flash chromatography (10/1 dichloromethane/methanol with 1% triethyl amine) to provide 1-(2-phenyl-piperazin-1-yl)-ethanone (200 mg, 119%). (M+H)+=205 m/e.

1. concentrationthe reaction mixture was concentrated in vacuo
2. additionThe residue was diluted with dichloromethane and silica-bound carbonate (2 g, 0.77 mmol/g, Silicycle, Inc.)
3. additionwas added
4. stirringThe reaction mixture was stirred overnight
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography (10/1 dichloromethane/methanol with 1% triethyl amine)