反应详情

温度

0 °C

10.51 g (53.9 mmol) of bromoacetic acid-tert-butyl ester is added in drops to a mixture of 10 g (21.55 mmol) of 1H,1H,2H,2H-perfluorodecan-1-ol and 0.73 g (2.15 mmol) of tetrabutylammonium hydrogen sulfate in 100 ml of 60% potassium hydroxide solution/50 ml of toluene while being stirred vigorously at 0° C. It is stirred for 1 hour at 0° C. 200 ml of toluene is added, the aqueous phase is separated and extracted twice with 50 ml of toluene each. The combined organic phases are dried on magnesium sulfate and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel (mobile solvent: hexane/dichloromethane/acetone=20/10/1).

1. stirringIt is stirred for 1 hour at 0° C
2. customthe aqueous phase is separated
3. extractionextracted twice with 50 ml of toluene each
4. customThe combined organic phases are dried on magnesium sulfate
5. concentrationconcentrated by evaporation in a vacuum
6. customThe residue is chromatographed on silica gel (mobile solvent: hexane/dichloromethane/acetone=20/10/1)