反応 #48608

反応方程式

2-(2-fluorophenyl)-ethanol

vinyl acetate

sodium carbonate

→

title compound

収率 72.2%

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

収率 72.2%

溶媒

toluene

反応条件

後処理

1. 1
   温度Cool the reaction mixture to room temperature
2. 2
   ろ過Vacuum filter the resultant slurry
3. 3
   その他to remove inorganic precipitates
4. 4
   洗浄washing the collected solid with hexanes
5. 5
   濃縮Concentrate
6. 6
   その他purify
7. 7
   洗浄(silica gel chromatography, eluting with hexanes)

実験手順

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%).

出典