反应详情

Under a nitrogen atmosphere, to a diethyl ether solution (175 mL) of 1-bromo-3,5-di-tert-butylbenzene (35.00 g, 130.00 mmol), a 1.65 M hexane solution of n-butyllithium (88.67 mL, 143.00 mmol) was added dropwise at −78° C. After the mixture was gradually warmed to room temperature, stirring was performed at room temperature for 2 hours. The resultant mixture was added dropwise to a solution of tetrachlorosilane (66.26 g, 390.00 mmol) dissolved in diethyl ether (58 mL) at −78° C. After the mixture was gradually warmed to room temperature, stirring was performed at room temperature for 3 hours. After completion of the reaction, the solvent was removed under reduced pressure. Thereafter, hexane was added to the residue, and insoluble materials were removed by filtration. The solvent was removed from the filtrate under reduced pressure. Purification by distillation under reduced pressure afforded trichloro(3,5-di-tert-butylphenyl)silane (24.11 g, yield 57.3%).

1. temperatureAfter the mixture was gradually warmed to room temperature
2. stirringstirring
3. waitwas performed at room temperature for 3 hours
4. customAfter completion of the reaction
5. customthe solvent was removed under reduced pressure
6. additionThereafter, hexane was added to the residue, and insoluble materials
7. customwere removed by filtration
8. customThe solvent was removed from the filtrate under reduced pressure
9. customPurification
10. distillationby distillation under reduced pressure