反应详情

温度

60 °C

Under a nitrogen atmosphere, 1-chloro-1-methyl-2,2-diphenylcyclopropane (2.43 g, 10.0 mmol), magnesium (0.279 g, 11.5 mmol) and THF (10 ml) were placed in a reaction flask, followed by addition of a trace amount of iodine and stirring at 60° C. for 5 hours. After cooling, copper iodide (1.92 g, 10.0 mmol), lithium bromide (0.879 g, 10.1 mmol) and chlorodi-tert-butylphosphine (2.1 ml, 11.0 mmol) were added and the resulting mixture was stirred at 60° C. for 3 hours, followed by cooling to room temperature. The resulting mixture was diluted with hexane (20 ml) and crystal separated was collected by filtration. The crystal was dissolved in toluene, and the toluene solution was washed with a 28% (w/w) aqueous ammonia and a brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (0.89 g, 25%) as white crystal.

1. temperatureAfter cooling
2. stirringthe resulting mixture was stirred at 60° C. for 3 hours
3. temperatureby cooling to room temperature
4. customseparated
5. filtrationwas collected by filtration
6. dissolutionThe crystal was dissolved in toluene
7. washthe toluene solution was washed with a 28% (w/w) aqueous ammonia
8. dry with materiala brine, and dried over anhydrous magnesium sulfate
9. customThe solvent was removed under reduced pressure