2,5-Dichlorophenethylamine was prepared as follows: to a solution of 2-(2,5-dichlorophenyl)acetonitrile (34.5 g, 185 mmol) in MeOH (1700 mL) was added NiCl2•6H2O (4.45 g, 18.7 mmol) at 0 C. After 10 min, solids from the initial green suspension were introduced into the solution. Methyl chloroformate (38.4 g, 406 mmol) was added via syringe over 10 min and then NaBH4 (41.4 g, 1.09 mol) was added in 8 small portions over 30 min at 0 C. Evolution of gas was observed and the reaction mixture turned black. After addition, the resulting mixture was stirred at 20 C for 1 h. LCMS analysis detected 48% yield of the desired product and 32% yield of 2,5-dichlorophenethylamine.
