反应详情

Under a nitrogen atmosphere, to a diethyl ether solution (106 mL) of 1-bromo-3,5-di-tert-butylbenzene (10.60 g, 39.37 mmol), a 1.65 M hexane solution of n-butyllithium (23.86 mL, 39.37 mmol) was added dropwise at −78° C. After the mixture was gradually warmed to room temperature, stirring was performed at room temperature for 3 hours. The resultant mixture was added dropwise to a diethyl ether solution (106 mL) of trichlorophenylsilane (24.99 g, 118.12 mmol) at −78° C. After the mixture was gradually warmed to room temperature, stirring was performed at room temperature. After completion of the reaction, the solvent was removed under reduced pressure. Thereafter, hexane wad added to the residue, and insoluble materials were removed by filtration. The solvent was removed from the filtrate under reduced pressure. Trichlorophenylsilane was removed by heating to 100° C. under reduced pressure to obtain dichloro(3,5-di-tert-butylphenyl)(phenyl)silane (11.77 g, yield 81.8%).

1. temperatureAfter the mixture was gradually warmed to room temperature
2. stirringstirring
3. customwas performed at room temperature
4. customAfter completion of the reaction
5. customthe solvent was removed under reduced pressure
6. additionThereafter, hexane wad added to the residue, and insoluble materials
7. customwere removed by filtration
8. customThe solvent was removed from the filtrate under reduced pressure
9. customTrichlorophenylsilane was removed
10. temperatureby heating to 100° C. under reduced pressure