Реакция #1960503

Уравнение реакции

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

bromoethane

potassium carbonate

→

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

Растворители

ethyl methyl ketone

Условия реакции

Обработка

1. 1
   ФильтрацияThe batch is filtered
2. 2
   Промывкаthe residue is washed with ethyl methyl ketone
3. 3
   КонцентрированиеThe filtrate is concentrated
4. 4
   ПромывкаThe solution is washed with water and sat. sodium chloride soln
5. 5
   Другоеand dried
6. 6
   Другоеafter removal of the solvent
7. 7
   Другоеis purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

Методика

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.

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