反应详情

In a flame dried round-bottomed flask equipped with a magnetic stir bar, a suspension of tert-butyl 4-(2-ethoxy-2-oxoethylidene)-3,3-difluoropiperidine-1-carboxylate (462 mg, 1.51 mmol) and Pd/C (10%, 70 mg) in dry EtOH (8 mL) was stirred at rt under a H2 atmospheric pressure until completion of the reaction. The mixture was then filtered, washed with EA/EtOH, and the filtrate concentrated under reduced pressure. The crude residue was purified by FC (hept-EA, 1:0→1:1) and the title compound obtained as a colorless oil. LC-MS-conditions 08: tR=0.89 min; [M-CH3+H]+=293.29.

1. customIn a flame dried round-bottomed flask equipped with a magnetic stir bar
2. customuntil completion of the reaction
3. filtrationThe mixture was then filtered
4. washwashed with EA/EtOH
5. concentrationthe filtrate concentrated under reduced pressure
6. customThe crude residue was purified by FC (hept-EA, 1:0→1:1)