反应详情

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).

1. customInto a 2 l four-necked flask equipped with a thermometer, a stirrer, a dropping funnel
2. customfurther reacted at from 20 to 30° C. for one hour
3. customreacted at from 80 to 90° C. for one hour
4. customAfter completion of the reaction
5. customprecipitated crystals
6. filtrationwere collected by filtration under reduced pressure
7. washwashed with water
8. washThen, the crystals were washed
9. custompurified at 20° C. by means of 500 ml of isopropyl alcohol
10. customdried with hot air