反应详情

温度

-10 °C

A suspension of 25.6 g (0.11 mol) 4-bromo-2-(trifluoromethyl)-aniline in 125 ml of conc. hydrochloric acid is cooled to −10° C. and a solution of 7.7 g (0.11 mol) sodium nitrite in 125 ml of water is added. The reaction mixture is stirred for 3 hours at −10 to −5° C., then a solution of 103 g (0.46 mol) tin-(II)-chloride-dihydrate in 125 ml of conc. hydrochloric acid is added dropwise. The mixture is stirred for 1 hour at −5° C. The precipitate formed is suction filtered and washed with water. The aqueous mother liquor is extracted with petroleum ether, then made basic with sodium hydroxide. The precipitate formed is extracted with diethyl ether. The organic phase is dried and evaporated to dryness. Yield: 12.9 g

1. stirringThe mixture is stirred for 1 hour at −5° C
2. customThe precipitate formed
3. filtrationfiltered
4. washwashed with water
5. extractionThe aqueous mother liquor is extracted with petroleum ether
6. customThe precipitate formed
7. extractionis extracted with diethyl ether
8. customThe organic phase is dried
9. customevaporated to dryness