Benzoyl chloride → 2,2,3,3,3-pentafluoro-1-phenylpropan-1-one

Temperature

0 °C

Firstly, the starting material was prepared as follows: under protective gas, 35 g (0.25 mol) of benzoyl chloride in 150 ml of CH2Cl2 were initially introduced at about -20° C. into a round-bottomed flask. 67 g (0.27 mol) of pentafluoroethyl iodide were firstly condensed in and 66.7 g (0.27 mol) of phosphorous acid trisdiethylamide were then metered in. The reaction mixture was subsequently stirred at 0° C. for a further 5 hours. After addition of the same volume of hexane to the reaction mixture, 2 phases formed. After phase separation, the lower phase was carefully extracted using hexane; the combined hexane phases were concentrated and distilled under reduced pressure. 20.8 g (58% yield) of pentafluoroethyl phenyl ketone of b.p. 76°-77° C./40 mbar were obtained.

1. customFirstly, the starting material was prepared
2. customformed
3. customAfter phase separation
4. extractionthe lower phase was carefully extracted
5. concentrationthe combined hexane phases were concentrated
6. distillationdistilled under reduced pressure

ORD record

ord-6566bfc97a014fb995da0d39d13b4d5e

Source dataset

uspto-grants-1991_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05017719