반응 #1960504

반응 방정식

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

caesium fluoride

→

7-ethoxy-1,2-difluoronaphthalene

용매

water

DMF

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   추출extracted a number of times with MTBE
3. 3
   세척The combined organic phases are washed with water and sat. sodium chloride soln
4. 4
   기타, and the solution is dried
5. 5
   기타after removal of the solvent
6. 6
   기타is purified by column chromatography (SiO2, toluene:ethyl acetate=9:1)

실험 절차

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.

출처