반응 #40336

반응 방정식

trimethylchlorosilane

4-phenylcyclohexanone

sodium iodide

triethylamine

→

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

수율 73.0%

용매

pentane

hexane

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONare added
2. 2
   추출The aqueous phase is extracted with hexane
3. 3
   세척The combined organic phases are washed with ice water
4. 4
   건조dried over sodium sulphate
5. 5
   기타the solvent is removed in a vacuum

실험 절차

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]+.

출처