반응 #1960503

반응 방정식

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

bromoethane

potassium carbonate

→

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

용매

ethyl methyl ketone

반응 조건

후처리

1. 1
   여과The batch is filtered
2. 2
   세척the residue is washed with ethyl methyl ketone
3. 3
   농축The filtrate is concentrated
4. 4
   세척The solution is washed with water and sat. sodium chloride soln
5. 5
   기타and dried
6. 6
   기타after removal of the solvent
7. 7
   기타is purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

실험 절차

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.

출처