反应详情

温度

23 °C

Commercially available 5-chloro-2-nitro-4-trifluoromethyl-phenylamine [CAS-No. 35375-74-7] (72.2 g, 300 mmol) was dissolved in DMSO (600 mL) and 2,2,2-trifluoroethanol (270 mL) were added at 23° C., the slightly exothermic reaction was cooled with a ice bath. KOH (85%, 99.0 g, 1500 mmol) were added slowly and the dark red reaction mixture was stirred at 23° C. for 4 days. Transferred into a 3 L flask and 1500 mL H2O were added under ice bath cooling, acidified with 3 N HCl and stirred at 23° C. for 3 h, filtered off the yellow precipitate, washed with H2O and dried in air at 60° C. to give the title compound as a yellow solid (89.47 g, 98%). MS (ISN) 303.1 [M·H].

1. customthe slightly exothermic reaction
2. temperaturewas cooled with a ice bath
3. customthe dark red reaction mixture
4. temperaturecooling
5. stirringstirred at 23° C. for 3 h
6. filtrationfiltered off the yellow precipitate
7. washwashed with H2O
8. customdried in air at 60° C.