HRID1429121

反应详情

EQUATION

反应方程式

HRID 1429121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, to a diethyl ether solution (70 mL) of dichloro(3,5-di-tert-butylphenyl)(phenyl)silane (7.00 g, 19.16 mmol), a solution of 3,5-dimethylphenyllithium (2.15 g, 19.16 mmol) dissolved in diethyl ether (22 mL) was added dropwise at −20° C. After the mixture was gradually warmed to room temperature, stirring was performed at room temperature. 3,5-Dimethylphenyllithium (1.26 g, 11.24 mmol) was added and further stirred at room temperature. 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 to obtain chloro(3,5-di-tert-butylphenyl)(3,5-dimethylphenyl)(phenyl)silane (7.21 g, yield 86.5%) as yellow oil.

WORKUP

后处理

  1. additionwas added dropwise at −20° C
  2. customwas performed at room temperature
  3. stirringfurther stirred at room temperature
  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