Water → 3,5-Dichloro-4-(2-(dimethylamino)acetamido)-benzylamine

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

Step F (3): To a solution of the compound of step F (2) (6 g 0.014 mol) in dry DMF (60 ml) under N2, anhydrous K2CO3 (6.03 g, 0.043 mol) was added with stirring. The reaction mixture was cooled to 0° C. and N,N-dimethylamine hydrochloride (2.37 g, 0.029 mol) was added at once. The reaction mixture was allowed stir for overnight at room temperature. The reaction mixture was poured into water and extracted with ethyl acetate (2×150 ml). The organic layer was washed with water (25 ml), brine (25 ml), dried over anhydrous sodium sulfate and concentrated under vacuum to remove the volatiles. The resulting crude product was purified by column chromatography using CHCl3: MeOH (9:1) as eluent to afford the product as an off-white solid (4 g, 72.9%)

Herkunft & Nachweise