反应详情

Intermediate 19 (2.6 g, 8.8 mmol) was added to a stirring solution of benzyl piperazine-1-carboxylate (1.1 mL, 5.87 mmol) in CH3CN (80 mL). The reaction mixture was refluxed over night, cooled, and quenched with satd. NaHCO3 (100 mL). The aqueous layer was extracted with EtOAc (3×50 mL) and the combined organic layers were washed with brine, dried over Na2SO4, concentrated to give the crude (3.8 g) as opaque oil. The chromatography (1:3, hexanes/EtOAc) afforded the title compound (1.78 g, 70%) as clear oil. ES/MS calcd. for C24H43N2O3Si+ 435.3. Found m/z=435.2 (M+H)+.

1. temperatureThe reaction mixture was refluxed over night
2. temperaturecooled
3. customquenched with satd
4. extractionThe aqueous layer was extracted with EtOAc (3×50 mL)
5. washthe combined organic layers were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated
8. customto give the crude (3.8 g) as opaque oil