Reaktion #214268

Reaktionsgleichung

trimethylchlorosilane

imidazole

1-ethynylcyclohexan-1-ol

dimethylformamide

→

product

1-Ethynyl-1-trimethylsilyloxycyclohexane

Lösungsmittel

hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith cooling in an ice bath
2. 2
   Temperaturwith cooling
3. 3
   workup.STIRRINGThe mixture is stirred for one hour
4. 4
   workup.WAITto stand overnight
5. 5
   SonstigeThe lower layer is separated
6. 6
   workup.ADDITIONdiluted with water
7. 7
   Extraktionextracted with hexane
8. 8
   WaschenThe hexane layers are washed several times with water
9. 9
   Trocknendried over magnesium sulfate
10. 10
    FiltrationFiltration
11. 11
    Sonstigeevaporation of the hexane-

Vorschrift

A 194 g portion of imidazole and 158.2 g of 1-ethynylcyclohexan-1-ol are mixed with 500 g of dimethylformamide with cooling in an ice bath. A 152 g portion of trimethylchlorosilane is added with cooling and stirring in about one minute. The mixture is stirred for one hour and allowed to stand overnight. One liter of hexane is added. The lower layer is separated, diluted with water and extracted with hexane. The hexane layers are washed several times with water and then combined and dried over magnesium sulfate. Filtration and then evaporation of the hexane-gives 198.5 g of product which is distilled giving 168 g of the desired product.

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