反应详情

To 1.0 g (6.36 mmol)of 2,3,6-trifluorobenzonitrile dissolved in 10 mL DMF was added 1.05 g (1.2 eq., 7.63 mmol) potassium carbonate and 1.18 g (1 eq., 6.36 mmol) piperazine-1-carboxylic acid tert-butyl ester. The mixture was stirred 30 minutes to completion, partitioned between ethyl acetate and water, dried over magnesium sulfate and concentrated under reduced pressure. Column chromatography, eluting with ethyl acetate/hexanes provided 665 mg of 4-(2-cyano-3,6-difluoro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester.

1. custompartitioned between ethyl acetate and water
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. washColumn chromatography, eluting with ethyl acetate/hexanes