反应详情

HOBt (290 mg, 2.14 mmol), DIEA (461 mg, 3.5 mmol), EDCI.HCl (410 mg, 2.14 mmol) followed by piperazine-1-carboxylic acid tert-butyl ester (398 mg, 2.14 mmol) were added to a stirred solution of 3-fluorobenzoic acid (250 mg, 1.78 mmol) in DMF (3 mL). The reaction mixture was stirred overnight and then diluted with cold water. The product was extracted with ethyl acetate and the organic layer was washed with brine solution, dried over Na2SO4, and concentrated under reduced pressure to afford 590 mg (92%) of 4-(3-fluoro-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester.

1. extractionThe product was extracted with ethyl acetate
2. washthe organic layer was washed with brine solution
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure