General procedure for the synthesis of N-methyl-2,2,2-trifluoroacetamide hydrochloride from N-methyl-2,2,2-trifluoroacetamide: A solution was prepared by dissolving lithium aluminum hydride (69 g, 1.8 mol) in 100 mL of ether at 100 °C. To this solution, an ether solution of 2,2,2-trifluoro-N-methylacetamide (86 g, 0.6 mol) was slowly added at 0 °C. The reaction mixture was stirred at room temperature overnight. Subsequently, sodium sulfate decahydrate was added to the mixture at -10°C and the resulting suspension was filtered. Dry HCl gas was passed into the filtrate until a white solid precipitated. The solid product was separated by filtration and recrystallized with a solvent mixture of methanol/ether to give N-methyl-2,2,2-trifluoroethylamine hydrochloride as a final white solid (73 g, 80.7% yield).
