تفاعل #1960503

معادلة التفاعل

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

bromoethane

potassium carbonate

→

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

المذيبات

ethyl methyl ketone

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe batch is filtered
2. 2
   غسيلthe residue is washed with ethyl methyl ketone
3. 3
   تركيزThe filtrate is concentrated
4. 4
   غسيلThe solution is washed with water and sat. sodium chloride soln
5. 5
   أخرىand dried
6. 6
   أخرىafter removal of the solvent
7. 7
   أخرىis purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

الإجراء التجريبي

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.

المصدر