反应详情

Oxalyl chloride (4.95 g, 39.0 mmol) was added dropwise to a mixture of 7-chloro-1-(cyclohexyl)methyl-1H-indole-3-carboxylic acid (6.4 g, 21.9 mmol) and dichloromethane (150 ml) under ice-water cooling and the resulting mixture was stirred at room temperate for 20 h. Dichloromethane and excess oxalyl chloride were removed by evaporation and the obtained residue was mixed with dichloromethane (100 ml). Aqueous ammonia (33%, 50 ml) and potassium carbonate (6.05 g, 43.8 mmol) was added into the mixture under ice-water bath cooling. After stirring at room temperature for 2 h, the reaction mixture was concentrated in vacuo, then the obtained solid was washed with water, then n-heptane, and dried under reduced pressure to afford 7-chloro-1-(cyclohexyl)methyl-1H-indole-3-carboxylic acid amide (6.4 g, 22.0 mmol).

1. customDichloromethane and excess oxalyl chloride were removed by evaporation
2. additionthe obtained residue was mixed with dichloromethane (100 ml)
3. temperaturecooling
4. stirringAfter stirring at room temperature for 2 h
5. concentrationthe reaction mixture was concentrated in vacuo
6. washthe obtained solid was washed with water
7. dry with materialn-heptane, and dried under reduced pressure