HRID1627412

反应详情

EQUATION

反应方程式

HRID 1627412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

THF in a volume of 100 ml was added to 6 g (49 mmol) of n-butylcyclopentadiene, and the mixture was cooled to −78° C. A 1.65 M hexane solution of n-butyllithium in a volume of 29.6 ml (48.8 mmol) was added thereto dropwise. The mixture was stirred at room temperature for 2 hours and was cooled again to −78° C. Dichloro(chloromethyl)(methyl)silane in an amount of 8.0 g (49 mmol) dissolved in 50 ml of THF was added dropwise. The mixture was stirred at room temperature for 3 hours and was concentrated under reduced pressure. Hexane was added, and the mixture was filtered. The filtrate was distilled under reduced pressure to give 3.43 g of target chloro(chloromethyl) (cyclopentadienyl)(methyl) silane.

WORKUP

后处理

  1. temperaturewas cooled again to −78° C
  2. additionwas added dropwise
  3. stirringThe mixture was stirred at room temperature for 3 hours
  4. concentrationwas concentrated under reduced pressure
  5. additionHexane was added
  6. filtrationthe mixture was filtered
  7. distillationThe filtrate was distilled under reduced pressure