反应详情

温度

-80 °C

To a solution of 38.5 g (0.225 mol) of 4-bromotoluene in 450 mL of THF, 300 mL (0.450 mol) of 1.5 M tBuLi in pentane was added dropwise with vigorous stirring for 2 hr at −80° C. This mixture was slowly warmed to room temperature and additionally stirred at this temperature for 30 min. To this mixture 52.0 g (0.23 mol) of 3-bromo-N,N-dimethylbenzamide was added at 0° C., and then this mixture was stirred for 12 hr at room temperature. Later, 300 mL of water was added, organic solvent was evaporated using a rotary evaporator. The product was extracted with 2×200 mL of dichloromethane. The combined organic extracts were evaporated to dryness, and the residue was dried in vacuum. This procedure gave 51.3 g (83%) of 40 which was further used without additional purification.

1. temperatureThis mixture was slowly warmed to room temperature
2. stirringadditionally stirred at this temperature for 30 min
3. stirringthis mixture was stirred for 12 hr at room temperature
4. customorganic solvent was evaporated
5. customa rotary evaporator
6. extractionThe product was extracted with 2×200 mL of dichloromethane
7. customThe combined organic extracts were evaporated to dryness
8. customthe residue was dried in vacuum