反应详情

Freshly prepared (3-methyl-1-oxo-3,4-dihydro-1H-isochromen-6-yl)acetaldehyde was dissolved in DCM. To the solution was added Boc-piperazine (671 mg, 3.6 mmol) followed by sodium triacetoxyborohydride (1.91 g, 9.0 mmol), the reaction mixture was allowed to stir overnight before being quenched with 10 mL of MeOH. The excess solvent was removed and the residue was re-redissolved in DCM; washed with water and brine, dried with magnesium sulfate, filtered, concentrated and purified via MPLC (50-100% EtOAc/Hex) to afford tert-butyl 4-[2-(3-methyl-1-oxo-3,4-dihydro-1H-isochromen-6-yl)ethyl]piperazine-1-carboxylate.

1. custombefore being quenched with 10 mL of MeOH
2. customThe excess solvent was removed
3. dissolutionthe residue was re-redissolved in DCM
4. washwashed with water and brine
5. dry with materialdried with magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified via MPLC (50-100% EtOAc/Hex)