反应详情

温度

0 °C

NaH (60% dispersion in mineral oil, 0.3 g, 7.3 mmole) was washed with hexane then suspended in anhydrous DMF (16 mL). The mixture was cooled to 0° C. and methyl 4-methoxy-1H-indol-2-carboxylate (1.0 g, 4.87 mmole) was added. The mixture was stirred under argon for 10 min, then MeI (1.3 mL, 20 mmole) was added, and the thick slurry was stirred at RT for 2.5 hr. The reaction was quenched with 10% NH4Cl (2 mL) and concentrated. The residue was partitioned between H2O and Et2O, and the organic layer was dried over MgSO4 and concentrated to yield the title compound (1.03 g, 96%) as a white solid: MS (ES) m/e 220.2 (M+H)+.

1. stirringthe thick slurry was stirred at RT for 2.5 hr
2. customThe reaction was quenched with 10% NH4Cl (2 mL)
3. concentrationconcentrated
4. customThe residue was partitioned between H2O and Et2O
5. dry with materialthe organic layer was dried over MgSO4
6. concentrationconcentrated