反应详情

To a solution of 23.0 g. of 4'-amino-3'-trifluoromethylisobutyranilide in 150 ml. of glacial acetic acid and 100 ml. of water, while maintaining the mixture temperature at 10°-20° C., slowly add 17 ml. of concentrated sulfuric acid, cool the resulting mixture to about 0° C. and slowly add 8.5 g. of sodium nitrite in 15 ml. of water maintaining the temperature of the reaction at about 0° C. for 30 minutes. Add 50 g. of potassium iodide in 150 ml. of water and stir the resulting mixture for 1 hour. Filter, water-wash and dissolve the precipitate in 200 ml. of ether and remove the iodine by washing with a 10% sodium sulfite solution. Dry, remove the solvent, and recrystallize from carbon tetrachloride, obtaining the compound of this example, m.p. 143°-145° C.

1. additionAdd 50 g
2. filtrationFilter
3. washwater-wash
4. dissolutiondissolve the precipitate in 200 ml
5. customof ether and remove the iodine
6. washby washing with a 10% sodium sulfite solution
7. customDry
8. customremove the solvent
9. customrecrystallize from carbon tetrachloride
10. customobtaining the compound of this example, m.p. 143°-145° C.