反应详情

温度

0 °C

A 500 mg portion of 2-methyl-1H-indole-5-carbonitrile was dissolved in 5 ml of dichloromethane, and 27.0 ml of 1 M tin tetrachloride (a dichloromethane solution) was added dropwise thereto at 0° C., followed by stirring at 0° C. for 10 minutes. Then, 0.27 ml of acetyl chloride was added thereto at 0° C., followed by overnight stirring at room temperature. A 25 ml portion of a 2 M sodium hydroxide aqueous solution was added thereto at 0° C. to adjust the pH to 12, followed by stirring at 0° C. for 1 hour and extraction with a 20% methanol-chloroform mixed solvent. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure to obtain 607 mg of 3-acetyl-2-methyl-1H-indole-5-carbonitrile as a beige solid.

1. customat 0° C.
2. waitat 0° C., followed by overnight
3. stirringstirring at room temperature
4. customat 0° C.
5. stirringby stirring at 0° C. for 1 hour
6. extractionextraction with a 20% methanol-chloroform mixed solvent
7. washThe organic layer was washed with saturated brine
8. dry with materialdried over anhydrous sodium sulfate
9. customthe solvent was evaporated under a reduced pressure