反应详情

To a mixture of methyl 3-acetyl-1H-indole-6-carboxylate (0.92 g) and DMF (18 ml) was added sodium hydride (0.18 g) under ice-cooling, followed by stirring at room temperature for 0.5 hour. Next, methyl iodide (0.29 ml) was added thereto under ice-cooling, followed by stirring at room temperature for 5 hours. Then, water was added thereto under ice-cooling, followed by stirring at room temperature. The solid precipitated was collected by filtration, washed with water, and purified by silica gel column chromatography (hexane/THF=2:1→chloroform /THF=9:1) to obtain methyl 3-acetyl-1-methyl-1H-indole-6-carboxylate (0.98 g).

1. temperaturecooling
2. temperatureunder ice-cooling
3. stirringby stirring at room temperature for 5 hours
4. temperatureunder ice-cooling
5. stirringby stirring at room temperature
6. customThe solid precipitated
7. filtrationwas collected by filtration
8. washwashed with water
9. custompurified by silica gel column chromatography (hexane/THF=2:1→chloroform /THF=9:1)