Reaktion #1960503

Reaktionsgleichung

7,8-difluoro-3-trimethylsilanylnaphthalen-2-ol

bromoethane

potassium carbonate

→

(3-ethoxy-5,6-difluoronaphthalen-2-yl)trimethylsilane

Lösungsmittel

ethyl methyl ketone

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe batch is filtered
2. 2
   Waschenthe residue is washed with ethyl methyl ketone
3. 3
   EinengenThe filtrate is concentrated
4. 4
   WaschenThe solution is washed with water and sat. sodium chloride soln
5. 5
   Sonstigeand dried
6. 6
   Sonstigeafter removal of the solvent
7. 7
   Sonstigeis purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

Vorschrift

54.7 g (about 0.12 mol) of 7,8-difluoro-3-trimethylsilanylnaphthalen-2-ol are stirred at 80° C. for 19 h together with 19.5 ml (0.26 mol) of bromoethane and 34.5 g (0.25 mol) of potassium carbonate in 400 ml of ethyl methyl ketone. The batch is filtered, and the residue is washed with ethyl methyl ketone. The filtrate is concentrated, and the residue is taken up in MTBE. The solution is washed with water and sat. sodium chloride soln. and dried using sodium sulfate. The residue remaining after removal of the solvent is purified by column chromatography (SiO2, toluene:ethyl acetate=9:1), giving (3-ethoxy-5,6-difluoronaphthalen-2-yl)trimethylsilane as a dark-brown solid.

Quelle