反应详情

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.

1. filtrationThe batch is filtered
2. washthe residue is washed with ethyl methyl ketone
3. concentrationThe filtrate is concentrated
4. washThe solution is washed with water and sat. sodium chloride soln
5. customand dried
6. customafter removal of the solvent
7. customis purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)