反应详情

温度

30 °C

In a suspension of 26.6 g of KOH in 200 ml of dimethylformamide, 20.1 g of solid 5-bromoindole was incorporated while being stirred. The mixture was stirred for 50 minutes at room temperature, and 25.4 g of benzyl chloride was dropwise added to the mixture over a period of 16 minutes at a temperature of not higher than 30° C. The reaction mixture was maintained at 30° C. in an oil bath for 5 hours with stirring. After completion of the reaction, 200 ml of water was added and the thus-formed aqueous phase was extracted with 120 ml of ether three times. The thus-obtained organic phase was washed with water and dried over sodium sulfate overnight. The dried product was concentrated to dryness and then recrystallized from isopropyl ether to give 23.5 g of N-benzyl-5-bromoindole. The yield was 80% by mole.

1. stirringThe mixture was stirred for 50 minutes at room temperature
2. stirringwith stirring
3. additionwas added
4. extractionthe thus-formed aqueous phase was extracted with 120 ml of ether three times
5. washThe thus-obtained organic phase was washed with water
6. dry with materialdried over sodium sulfate overnight
7. concentrationThe dried product was concentrated to dryness
8. customrecrystallized from isopropyl ether