反应详情

Into a 1 l four-necked flask equipped with a thermometer, a stirrer, a dropping funnel and a N2 gas supply tube, a N2 gas was introduced so that the interior of the flask became a N2 atmosphere. 250 ml of dimethylformamide and 16.5 g (0.426 mol) of sodium hydride (62% oil suspension) were charged, and a solution comprising 69 g (0.387 mol) of 2-(4-fluorophenyl)-2-(N,N-dimethylamino)acetonitrile and 75.4 g (0.387 mol) of 4-(trifluoromethyl)benzyl chloride, was dropwise added over a period of one hour at from 10 to 15° C. under cooling with ice water and then further reacted at from 20 to 30° C. for one hour. Then, 280 ml of 40% sulfuric acid was added to this reaction mixture and reacted at from 80 to 90° C. for one hour. After completion of the reaction, 2 l of water was added, and precipitated crystals were collected by filtration and washed with a 2% sodium hydrogen carbonate aqueous solution and water. Then, the crystals were further washed and purified with 100 ml of n-hexane and then vacuum-dried to obtain 97.7 g (yield: 89.4%) of the desired compound (melting point: 93-95° C.) as slightly yellow crystals.

1. customInto a 1 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. additionwas added
5. customprecipitated crystals
6. filtrationwere collected by filtration
7. washwashed with a 2% sodium hydrogen carbonate aqueous solution and water
8. washThen, the crystals were further washed
9. custompurified with 100 ml of n-hexane
10. customvacuum-dried