Synthesis
The reaction was carried out in anhydrous ethanol (50 mL) at reflux for 45 minutes with 4-amino-3-nitrobenzotrifluoride (5.000 g, 24.26 mmol, Aldrich, direct use) and SnCl2-2H2O (20.00 g, 88.64 mmol, Aldrich, direct use). Upon completion of the reaction, the mixture was poured into ice (85 g) and alkalized with 10% aqueous NaHCO3 (250 mL). Subsequently, the resulting suspension was extracted with ethyl acetate (400 mL). The ethyl acetate extracts were combined, dried with Na2SO4, and the solvent was evaporated under reduced pressure to give 4.14 g (87% yield) of pure 4-trifluoromethyl-1,2-phenylenediamine as a red powder.
