Hydroxylamine HCl → HCID 59115139, compound

Participants

Reaction Steps

49.3 g (224 mmol) of 2,2,2-trifluoro-1-(4-methylsulfanyl-phenyl)-ethanone are dissolved in 250 ml of hot ethanol. To this solution is added dropwise a solution of hydroxylammonium chloride (16.3 g, 235 mmol) and sodium acetate (31.2 g, 381 mmol) in 125 ml of water, and the reaction solution is stirred under reflux for 6.5 hr. The reaction mixture was concentrated by rotary evaporation and poured into ice/water. The resulting yellow solid is filterd and washed with water. After drying under reduced pressure, recrystallization from hexane-ethyl acetate affords 28.4 g of white solid (54%). The structure is confirmed by the 1H-NMR spectrum (CDCl3), δ[ppm]:: d 2.51 (s, 3H), 7.31 (d, 2H), 7.49 (d, 2H), 8.80 (broad s, 1H).

Provenance & Evidence