Nitrogen → 4'-Fluoro-2-(4-trifluoromethylphenyl)acetophenone

Beteiligte Stoffe

Reaktionsschritte

Into a 2 l four-necked flask equipped with a thermometer, a stirrer, a dropping funnel and a N2 gas supply tube, a N2 gas was supplied so that the interior of the flask became a N2 atmosphere. 400 ml of dimethylformamide and 35.0 g (0.9 mol) of sodium hydride (62% oil suspension) were charged, and a mixed solution comprising 133.5 g (0.75 mol) of 2-(4-fluorophenyl)-2-(N,N-dimethylamino)acetonitrile, 145.9 g (0.75 mol) of 4-(trifluoromethyl)benzyl chloride and 280 ml of dimethylformamide, was dropwise added over a period of one hour at from 10 to 25° C. under cooling with water and then further reacted at from 20 to 30° C. for one hour. Then, 330 g of 40% sulfuric acid aqueous solution was added to this reaction mixture and reacted at from 80 to 90° C. for one hour. After completion of the reaction, the reaction product was added to 2 e of water, and precipitated crystals were collected by filtration under reduced pressure and washed with water. Then, the crystals were washed and purified at 20° C. by means of 500 ml of isopropyl alcohol and then dried with hot air to obtain 204.7 g (yield: 95.2%) of the desired compound having a purity of 98.4% (by HPLC analysis).

Herkunft & Nachweise