反応 #1960503

反応方程式

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

bromoethane

potassium carbonate

→

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

溶媒

ethyl methyl ketone

反応条件

後処理

1. 1
   ろ過The batch is filtered
2. 2
   洗浄the residue is washed with ethyl methyl ketone
3. 3
   濃縮The filtrate is concentrated
4. 4
   洗浄The solution is washed with water and sat. sodium chloride soln
5. 5
   その他and dried
6. 6
   その他after removal of the solvent
7. 7
   その他is purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

実験手順

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.

出典