The general procedure for the synthesis of 3,5-bis(trifluoromethyl)benzenemethanamine from 3,5-bis(trifluoromethyl)benzaldehyde was as follows: to a 300 mL autoclave was added 145.3 g (0.60 mol) of 3,5-bis(trifluoromethyl)benzenemethanaldehyde and 60 mL of cooled ethanol solution containing 10.3 g (0.60 mol) of liquid ammonia, followed by the addition of 2 g of nickel ruanide. The mixture was heated to 40 °C and the reaction was stirred under hydrogen pressure (9 MPa) for 1 hour. The temperature was then raised to 70 °C and the reaction was continued for 30 min. Upon completion of the reaction, the reaction product solution was drained and filtered to remove the catalyst. Analysis of the reaction solution by gas chromatography confirmed the formation of 128.9 g (0.53 mol) of 3,5-bis(trifluoromethyl)benzylamine in 89% yield and 93% selectivity. 124.0 g (0.51 mol) of 3,5-bis(trifluoromethyl)benzylamine was isolated by vacuum distillation in 85% yield, and the purity determined by gas chromatography was ≥99%.The results of ICP analysis of the total elements showed that Li, Na, K, Mg, Ca, Sr, Ba, Sc, Y, Ti, Zr, V, Nb, Cr, Mo, W, Mn, Fe, Ru, Co were not detected; Rh, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, In, Si, Sn, Pb, P, Sb, and S were detected, and the contents of group 1 and group 2 elements were ≤1 ppm.
