反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas cooled again to −78° C
- additionwas added dropwise
- stirringThe mixture was stirred at room temperature for 3 hours
- concentrationwas concentrated under reduced pressure
- additionHexane was added
- filtrationthe mixture was filtered
- distillationThe filtrate was distilled under reduced pressure