反应详情

To an ice-cooled solution of 2,2-dimethylpropionic acid 2-((R)-3-aminopiperidin-1-yl)ethyl ester (1.675 g, 7.33 mmol) in DMF (30 mL) was added 2,4-difluoronitrobenzene (1.517 g, 9.54 mmol) and potassium carbonate (2.03 g, 14.7 mmol). The reaction mixture was stirred at RT for 16 h, then partitioned between water and EtOAc. The aqueous phase was extracted with EtOAc and the combined organic fractions washed with water, followed by brine, then dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, eluant 10-40% EtOAc in cyclohexane) affording the title compound as a yellow oil (2.533 g, 94%). LCMS (Method J): RT 2.31 min [M+H]+ 368.

1. custompartitioned between water and EtOAc
2. extractionThe aqueous phase was extracted with EtOAc
3. washthe combined organic fractions washed with water
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by column chromatography (Si—PCC, eluant 10-40% EtOAc in cyclohexane)