تفاعل #1960504

معادلة التفاعل

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

caesium fluoride

→

7-ethoxy-1,2-difluoronaphthalene

المذيبات

water

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   استخلاصextracted a number of times with MTBE
3. 3
   غسيلThe combined organic phases are washed with water and sat. sodium chloride soln
4. 4
   أخرى, and the solution is dried
5. 5
   أخرىafter removal of the solvent
6. 6
   أخرىis purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

الإجراء التجريبي

44.0 g (about 81.6 mmol) of (3-ethoxy-5,6-difluoronaphthalen-2-yl)trimethylsilane are stirred at 100° C. for 20 h together with 26.3 g (0.17 mol) of caesium fluoride in 300 ml of DMF. After cooling, the mixture is diluted with water and extracted a number of times with MTBE. The combined organic phases are washed with water and sat. sodium chloride soln., and the solution is dried using sodium sulfate. The brown oil remaining after removal of the solvent is purified by column chromatography (SiO2, toluene:ethyl acetate=9:1), giving 7-ethoxy-1,2-difluoronaphthalene as a brown oil.

المصدر