Reaktion #92001

Reaktionsgleichung

DMF

3,5-dichlorophenol

imidazole

triisopropylchlorosilane

→

(3,5-dichlorophenoxy)-triisopropylsilane

Ausbeute 97.4%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe organic compound was extracted into ethyl acetate (2×100 mL)
2. 2
   Waschenthe combined organic layer was washed with brine solution
3. 3
   Trocknendried over anhydrous MgSO4
4. 4
   FiltrationFiltration and concentration
5. 5
   Sonstigegave the crude residue which
6. 6
   Sonstigewas purified

Vorschrift

To a mixture of 3,5-dichlorophenol (16.3 g, 100 mmol), imidazole (14.98 g, 220 mmol), and triisopropylchlorosilane (21.21 g, 110 mmol) was added DMF (200 mL) at room temperature. The resulting brown solution was stirred for 15 h and then it was diluted with water (500 mL). The organic compound was extracted into ethyl acetate (2×100 mL) and the combined organic layer was washed with brine solution and dried over anhydrous MgSO4. Filtration and concentration gave the crude residue which was purified using an ISCO (400 g) column chromatography to obtain 31.1 g (97%) of (3,5-dichlorophenoxy)-triisopropylsilane as a colorless oil. EI(+)-HRMS m/e calcd. for C15H24Cl2OSi (M)+ 318.0973, obsd. 318.0971.

Quelle