反应详情

温度

0 °C

Sodium hydride (60% in mineral oil, 200 mg, 5 mmol) was added at 0° C. to a solution of 3-phenyl-1H-indole (1a) (940 mg, 4.86 mmol) in N,N-dimethylformamide (20 mL) under a nitrogen atmosphere. The suspension was stirred for 15 minutes at 0° C. and methyliodide (311 μL, 5 mmol) was then added. The reaction mixture was warmed to room temperature, stirred for 6 hours and then concentrated in vacuo. The residue was partitioned between ethyl acetate (30 mL) and water (10 mL). The organic layer was washed with water (2×10 mL), brine (10 mL), dried over sodium sulfate, filtered and evaporated to dryness to give the desired product (1b) as a yellow oil (1 g, 4.86 mmol, 100%) which was used without further purification.

1. temperatureThe reaction mixture was warmed to room temperature
2. stirringstirred for 6 hours
3. concentrationconcentrated in vacuo
4. customThe residue was partitioned between ethyl acetate (30 mL) and water (10 mL)
5. washThe organic layer was washed with water (2×10 mL), brine (10 mL)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. customevaporated to dryness