反应详情

To a solution of ethyl 5-(3-dimethylamino-piperidine-1-carbonyl)-1H-indole-2-carboxylate (1.51 g, 4 mmol) in acetonitrile (30 ml) were added isopropylmethane-sulfonate (1.8 eq, 1.1 g) and caesium carbonate (1.8 eq, 2.6 g). The mixture was heated overnight at reflux. The solvent was evaporated under reduced pressure and the residue partitioned between water and tert-butylmethyl ether. The phases were separated, the aqueous phase extracted with tert-butylmethyl ether and the combined organic phases washed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (4:1 chloroform/methanol eluant) to afford the product as a light-brown gum. (31%)

1. temperatureThe mixture was heated overnight
2. temperatureat reflux
3. customThe solvent was evaporated under reduced pressure
4. customthe residue partitioned between water and tert-butylmethyl ether
5. customThe phases were separated
6. extractionthe aqueous phase extracted with tert-butylmethyl ether
7. washthe combined organic phases washed with brine
8. dry with materialdried over magnesium sulfate
9. customevaporated under reduced pressure
10. customThe residue was purified by column chromatography on silica gel (4:1 chloroform/methanol eluant)