反应详情

The mixture of 4,4-dimethyl-7-nitro-1,2,3,4-tetrahydro-quinoline (0.48 g, 2.33 mmol), iodoethane (0.21 ml, 2.56 mmol), and NaH (60%, 0.10 g, 2.5 mmol) in 10 ml of DMF was stirred at RT overnight, and partitioned between EtOAc and H2O. The combined organic portions were washed with brine, dried with MgSO4, filtered, and condensed. The crude compound was purified by flash column chromatography (5 to 10% of CH2Cl2 in hexanes). The titled compound was obtained as a yellow oil. MS (ES+): 235.3 (M+H)+. Calc'd for C13H18N2O2—234.29.

1. custompartitioned between EtOAc and H2O
2. washThe combined organic portions were washed with brine
3. dry with materialdried with MgSO4
4. filtrationfiltered
5. customcondensed
6. customThe crude compound was purified by flash column chromatography (5 to 10% of CH2Cl2 in hexanes)