反应 #40336

反应方程式

trimethylchlorosilane

4-phenylcyclohexanone

sodium iodide

triethylamine

→

Trimethyl-(4-phenyl-cyclohex-1-enyloxy)-silane

收率 73.0%

溶剂

pentane

hexane

acetonitrile

反应条件

后处理

1. 1
   workup.ADDITIONare added
2. 2
   萃取The aqueous phase is extracted with hexane
3. 3
   洗涤The combined organic phases are washed with ice water
4. 4
   干燥dried over sodium sulphate
5. 5
   其他the solvent is removed in a vacuum

实验过程

sodium iodide (12.4 mmol) dissolved in acetonitrile (12.4 ml), is added dropwise at room temperature to a solution of 4-phenylcyclohexanone (10 mmol) in hexane (10 ml), followed by triethylamine (12.4 mmol) and trimethylchlorosilane (12.4 mmol). After stirring for two hours cold pentane and ice water are added. The aqueous phase is extracted with hexane. The combined organic phases are washed with ice water, dried over sodium sulphate and the solvent is removed in a vacuum. Trimethyl-(4-phenyl-cyclohex-1-enyloxy)-silane (1.8 g) is obtained in pure form in a yield of 73% (Tetrahedron 1987, 43, 9, 2075-2088): tR 2.29 min (LC-2); ESI-MS (+): m/z 247.27 [M+H]+.

来源