反应详情

温度

0 °C

1.28 ml of POCl3 was added dropwise to a solution of 3.24 g of ethyl 1-cyclopropyl-4-methoxy-1H-indole-6-carboxylate in 30 ml of DMF and the mixture was stirred at 0° C. for 2 hrs. The mixture was diluted with EtOAc and 25 ml of 1N NaOH was added. Then the mixture was made basic using saturated NaHCO3aq. The mixture was extracted with EtOAc and the extract was washed with water and saturated brine, dried over Na2SO4, then concentrated. The residue was purified on SiO2 column chromatography (EtOAc-n-Hexane system) to give 2.4 g of ethyl 1-cyclopropyl-3-formyl-4-methoxy-1H-indole-6-carboxylate.

1. additionwas added
2. extractionThe mixture was extracted with EtOAc
3. washthe extract was washed with water and saturated brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was purified on SiO2 column chromatography (EtOAc-n-Hexane system)