1-Bromo-4-iodobenzene → 1-Bromo-4-(pentafluoroethyl)benzene

Temperatur

80 °C

Under argon in a microwave vial 2 g 1-bromo-4-iodobenzene, 3.3 g trimethyl(perfluoroethyl)silane, 493 mg potassium fluoride and 2 g copper iodide are suspended in 10 ml N,N-dimethylformamide. The mixture is heated for 12 hours at 80° C. Further 3.3 g trimethyl(perfluoroethyl)silane are added and heating is continued for 48 hours. Then the mixture is partitioned between 2 M ammonia and diethylether. The aqueous phase is twice extracted with diethylether. The combined organic phases are washed three times with water and dried with magnesium sulphate. The solvent is evaporated in vacuo (300 mbar, temperature of water bath 50° C.). The residue is chromatographed on silica gel (dichloromethane).

1. temperatureheating
2. customThen the mixture is partitioned between 2 M ammonia and diethylether
3. extractionThe aqueous phase is twice extracted with diethylether
4. washThe combined organic phases are washed three times with water
5. dry with materialdried with magnesium sulphate
6. customThe solvent is evaporated in vacuo (300 mbar, temperature of water bath 50° C.)
7. customThe residue is chromatographed on silica gel (dichloromethane)

ORD-Eintrag

ord-46f52acc79b14cd694f7e805bd7512fc

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09029544B2