反应详情

To a solution of 4-(2-ethyl-6-fluoro-1H-indol-3-yl)piperidine-1-carboxylic acid tert-butyl ester (0.36 g) in degassed toluene (10 ml) at r.t., is added potassium phosphate (0.1 g), copper iodide (20 mg), iodobenzene (254 mg) and N,N′-dimethylcyclohexane-1,2-diamine (30 mg). The mixture is heated at reflux for 3 days. Thereafter the mixture is allowed to cool to r.t., and water (20 ml) added. Ethyl acetate (3×10 ml) is used to extract the organic components and the organic layer is washed with water, dried over MgSO4 and concentrated in vacuo. Flash chromatography (9:1 cyclohexane:ethyl acetate) gives 120 mg pure product (27%) as a brown solid.

1. temperatureThe mixture is heated
2. temperatureat reflux for 3 days
3. extractionto extract the organic components
4. washthe organic layer is washed with water
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo