반응 #48608

반응 방정식

2-(2-fluorophenyl)-ethanol

vinyl acetate

sodium carbonate

→

title compound

수율 72.2%

1-Fluoro-2-(2-vinyloxyethyl)-benzene

수율 72.2%

용매

toluene

반응 조건

후처리

1. 1
   온도Cool the reaction mixture to room temperature
2. 2
   여과Vacuum filter the resultant slurry
3. 3
   기타to remove inorganic precipitates
4. 4
   세척washing the collected solid with hexanes
5. 5
   농축Concentrate
6. 6
   기타purify
7. 7
   세척(silica gel chromatography, eluting with hexanes)

실험 절차

Combine 2-(2-fluorophenyl)-ethanol (3.08 g, 22.0 mmol), vinyl acetate (4 mL, 43.3 mmol), anhydrous toluene (22 mL), chloro(1,5-cyclooctadiene)iridium(I) dimer (155 mg, 0.231 mmol), and anhydrous sodium carbonate (1.5 g, 14.2 mmol) in a dry round-bottom flask fitted with a reflux condensor under a nitrogen atmosphere. Heat the resulting mixture to 95° C. for 5 hours. Cool the reaction mixture to room temperature. Vacuum filter the resultant slurry to remove inorganic precipitates, washing the collected solid with hexanes. Concentrate and purify (silica gel chromatography, eluting with hexanes) to give the title compound as a yellow oil (2.64 g, 72%).

출처