反应详情

Methyl lithium (1.59M solution in ether; 13.8 ml) was added dropwise to a stirred cold (-65° to -55°) solution of 1-methyl-1H-indole-4-carboxylic acid (1.75 g) in dry THF (50 ml) under nitrogen and stirring was continued while the mixture warmed to 0° over 2 h. The reaction was then quenched with saturated ammonium chloride solution (50 ml) and the layers were separated. The aqueous layer was further extracted with dichloromethane (2×50 ml) and the combined organic layers were washed with brine (2×50 ml), dried and evaporated in vacuo. The residual solid (1.8 g) was purified by FCC eluting with dichloromethane to give the title compound (1.6 g), m.p. 63°-64°.

1. temperaturewarmed to 0° over 2 h
2. customThe reaction was then quenched with saturated ammonium chloride solution (50 ml)
3. customthe layers were separated
4. extractionThe aqueous layer was further extracted with dichloromethane (2×50 ml)
5. washthe combined organic layers were washed with brine (2×50 ml)
6. customdried
7. customevaporated in vacuo
8. customThe residual solid (1.8 g) was purified by FCC
9. washeluting with dichloromethane