反应详情

温度

0 °C

A solution of 6-methylsulfanyl-1H-indole (6.8 g, 42 mmol) in DMF (50 mL) was added to a slurry of NaH (55 mmol) in DMF(10 mL) at 0° C. over a period of 10 minutes. After stirring for 1 hour at 0° C., CH3I (4.0 ml,64 mmol) was added and the mixture stirred for 30 minutes at 0° C., then at room temperature for 1 hour, then poured into ice/H2O and extracted with EtOAc. The organic phase was washed with saturated NaCl solution, dried over MgSO4, filtered and evaporated to give 6.7 g (91.0%) of 1-methyl-6-methylsulfanyl-1H-indole as a yellow oil after flash column chromatography.

1. stirringthe mixture stirred for 30 minutes at 0° C.
2. waitat room temperature for 1 hour
3. extractionextracted with EtOAc
4. washThe organic phase was washed with saturated NaCl solution
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated