反应详情

Into a solution of ethyl 6-(4-methylphenyl)-1H-indole-2-carboxylate (0.9 g) in DMF (10 ml) was added at 0° C. sodium hydride (60%, 0.14 g), and the resulting mixture was stirred for 15 minutes. Into the reaction mixture was added methyl iodide (0.22 ml), and the resulting mixture was stirred at room temperature for 3 hours. The reaction mixture was mixed with water and was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with magnesium sulfate. After concentration of the organic layer under reduced pressure, the residue was subjected to separation and purification using column chromatography (ethyl acetate/hexane 1:4) and further to recrystallization (ethyl acetate/hexane) to obtain ethyl 1-methyl-6-(4-methylphenyl)-1H-indole-2-carboxylate (0.80 g) as colorless crystals.

1. stirringthe resulting mixture was stirred at room temperature for 3 hours
2. extractionwas extracted with ethyl acetate
3. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
4. dry with materialwas dried with magnesium sulfate
5. customAfter concentration of the organic layer under reduced pressure, the residue was subjected to separation and purification
6. customfurther to recrystallization (ethyl acetate/hexane)