反应详情

A solution of 20% TFA in DCM (25 mL) was added to 8-[3-(methyloxy)-4-nitrophenyl]-1,4-dioxaspiro[4.5]dec-7-ene (900 mg, 3.09 mmol) and the mixture was stirred at rt for approximately 14 h. The reaction was then concentrated under vacuum. The residue was dissolved in EtOAc and aqueous (saturated) NaHCO3. The organic layer was separated, washed with H2O, dried over MgSO4, filtered, then concentrated and purified by silica gel chromatography to give the title compound of step D (520 mg, 2.10 mmol, 68%) as a tan solid. MS (ESI): 248 [M+H]+.

1. concentrationThe reaction was then concentrated under vacuum
2. dissolutionThe residue was dissolved in EtOAc
3. customThe organic layer was separated
4. washwashed with H2O
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by silica gel chromatography