反应详情

Phosphorous oxychloride (1.9 mL, 20 mmol) was added to a suspension of 4-bromo-1H-indole-2-carboxylic acid amide (1.32 g, 5.5 mmol.) in toluene (10 mL) and the mixture was stirred at reflux for 45 min. On cooling, the mixture was poured into an aqueous Na2CO3 solution (sat., 50 mL) and the mixture stirred until effervescence had subsided. The layers were separated, the aqueous phase extracted with EtOAc and the combined organic layers dried (MgSO4) and evaporated to dryness. The crude material was purified by column chromatography to afford the title compound as a solid (1.00 g, 82%).

1. temperatureat reflux for 45 min
2. temperatureOn cooling
3. stirringthe mixture stirred until effervescence
4. customThe layers were separated
5. extractionthe aqueous phase extracted with EtOAc
6. dry with materialthe combined organic layers dried (MgSO4)
7. customevaporated to dryness
8. customThe crude material was purified by column chromatography