反应详情

To a stirred suspension of sodium hydride (0.27 g, 60% dispersion in mineral oil) in DMF (50 mL) under nitrogen at room temperature was added ethyl 4-benzyloxyindole-2-carboxylate (1.59 gm). Methyl iodide (0.5 mL) was added 10 min. later. After 2 hr. excess sodium hydride was quenched with acetic acid (0.4 mL) and the solvent evaporated under reduced pressure. The residue was taken into EtOAc, washed with water and brine, dried over MgSO4, and evaporated to dryness to give an oil which was triturated with hexane to precipitate 1.45 g of the title compound. Mp 89-90.5° C.

1. customexcess sodium hydride was quenched with acetic acid (0.4 mL)
2. customthe solvent evaporated under reduced pressure
3. washwashed with water and brine
4. dry with materialdried over MgSO4
5. customevaporated to dryness
6. customto give an oil which
7. customwas triturated with hexane
8. customto precipitate 1.45 g of the title compound