反应详情

温度

0 °C

To a suspension of NaH (0.146 g, 3.818 mmol, 60%) in DMF (20 ml) cooled at 0° C. was added 4-phenylpiperidine (0.616 g, 3.818 mmol). The resulting mixture was stirred for 5 min., then compound D1 (1 g, 3.016 mmol) was added. The resulting reaction mixture was stirred for 1 h. The reaction mixture was then quenched with NH4Cl (aqueous sat. solution) and extracted with Et2O. The organic layer was separated, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH gradient as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D6 (0.985 g, 75%).

1. customThe resulting reaction mixture
2. stirringwas stirred for 1 h
3. customThe reaction mixture was then quenched with NH4Cl (aqueous sat. solution)
4. extractionextracted with Et2O
5. customThe organic layer was separated
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH gradient as eluent)
9. customThe desired fractions were collected
10. concentrationconcentrated in vacuo