反应详情

温度

80 °C

A mixture of ethyl 1H-indole-2-carboxylate (5.68 g, 30 mmol), tert-butyl 2-bromoacetate (6.44 g, 33 mmol), and potassium carbonate in 60 mL of DMF was heated to 80° C. for 2 days. The TLC showed that the reaction stopped at around 50% completion. The reaction was worked up by the addition of water and the aqueous phase was extracted with EtOAc (2×30 mL). The combined organic phase was washed with brine, dried over Na2SO4, filtered and evaporated. The residue was purified by Combiflash (40 g silica gel cartridge, 0-30% EtOAc in hexane) to afford the desired product.

1. extractionthe aqueous phase was extracted with EtOAc (2×30 mL)
2. washThe combined organic phase was washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by Combiflash (40 g silica gel cartridge, 0-30% EtOAc in hexane)