反应详情

After tert-butyl 3-oxopiperidine-1-carboxylate (1 g, 5.02 mmol) was dissolved in THF (20 ml), and then trimethyl(trifluoromethyl)silane (0.5M solution in THF, 20 ml, 10.0 mmol) and tetrabutylammonium fluoride (1.0M solution in THF, 10.5 ml, 10.5 mmol) were sequentially added thereto at 0° C., followed by stirring at room temperature for 2 hours. A saturated aqueous ammonium chloride solution (5 ml) was added to the resulting reaction liquid, followed by stirring for 20 minutes. The resulting reaction liquid was concentrated under reduced pressure, and then MC (100 ml) was added to the residue thus obtained, followed by washing with distilled water (20 ml). The organic layer was dried over anhydrous magnesium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (20% EtOAc/Hexanes), to obtain 709 mg of white solid (53%).

1. customat 0° C.
2. stirringby stirring for 20 minutes
3. customThe resulting reaction liquid
4. concentrationwas concentrated under reduced pressure
5. additionMC (100 ml) was added to the residue
6. customthus obtained
7. washby washing with distilled water (20 ml)
8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
9. filtrationfollowed by filtration and concentration
10. customthe residue thus obtained