反应详情

Under ice-cooling, 1.3 ml of phosphorus oxychloride was added to 7 ml of N,N-dimethylformamide at an inner temperature of from 10 to 20° C., followed by stirring at room temperature for 15 minutes. Under ice-cooling, 9 ml of an N,N-dimethylformamide solution of 2-methyl-1H-indole-5-carbonitrile was added to this solution at an inner temperature of from 10 to 20° C., followed by overnight stirring at room temperature. A 64 ml portion of water was added thereto at 0° C. and the pH was adjusted to 8 with potassium carbonate, followed by 2.5 hours of stirring at room temperature. The thus precipitated solid was collected by filtration, washed with water and then dried at 80° C. under a reduced pressure to obtain 1.73 g of 3-formyl-2-methyl-1H-indole-5-carbonitrile as a pale yellow solid.

1. temperatureUnder ice-cooling
2. temperatureUnder ice-cooling
3. waitfollowed by overnight
4. stirringstirring at room temperature
5. customat 0° C.
6. waitfollowed by 2.5 hours
7. stirringof stirring at room temperature
8. filtrationThe thus precipitated solid was collected by filtration
9. washwashed with water
10. customdried at 80° C. under a reduced pressure