反应详情

5-Nitro-2-(tetrahydro-pyran-4-ylmethyl)-2H-isoquinolin-1-one (0.78 g, 0.0027 mol) and tin dichloride dihydrate (2 g, 0.01 mol) were stirred in tetrahydrofuran (10 mL, 0.1 mol) at room temperature for 24 hours. The mixture was partitioned between EtOAc (100 mL) and saturated aqueous NaHCO3 solution, separated. The aqueous layer was extracted with EtOAc (50 mL×3). The combined organic layers were dried over Na2SO4, and purified via flash chromatography (40 g of silica gel, 0-100% EtOAc/Hexanes) to give a yellow solid. MS m/z (M+H) 259.2.

1. customThe mixture was partitioned between EtOAc (100 mL) and saturated aqueous NaHCO3 solution
2. customseparated
3. extractionThe aqueous layer was extracted with EtOAc (50 mL×3)
4. dry with materialThe combined organic layers were dried over Na2SO4
5. custompurified via flash chromatography (40 g of silica gel, 0-100% EtOAc/Hexanes)
6. customto give a yellow solid