反应详情

(1-Oxo-3,4-dihydro-1H-isochromen-6-yl)acetaldehyde (2.40 g, 12.6 mmol) was combined with 1-Boc-piperazine (3.53 g, 18.9 mmol) and sodium triacetoxyborohydride (13.4 g, 63.1 mmol) in DCM (90 mL). The reaction mixture was stirred at room temperature overnight. Saturated sodium bicarbonate solution was added and the layers were separated. The organic layer was washed with brine, then dried over MgSO4. The crude product was purified first by MPLC (silica), eluting with 3% of a 10% NH4OH/methanol solution in DCM, then a second MPLC purification eluting with ethyl acetate, to afford the title compound. LCMS: m/z 361 (M+1)+.

1. customthe layers were separated
2. washThe organic layer was washed with brine
3. dry with materialdried over MgSO4
4. customThe crude product was purified first by MPLC (silica)
5. washeluting with 3% of a 10% NH4OH/methanol solution in DCM
6. customa second MPLC purification
7. washeluting with ethyl acetate