3,4,5-trichloro-1-oxidopyridin-1-ium

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Prepared according to the procedure described for example 17 from 3,4,5-trichloro-1-oxido-pyridin-1-ium (0.75 g, 3.8 mmol) and sodium hydrosulfide hydrate (0.38 g, 4.57 mmol). The title compound was obtained as a brown solid (0.52 g, 70% yield). 1H NMR (400 MHz, d6-DMSO) δ: 7.89 (2H, s). MS m/z: 195.9 [M+H]+. Prepared

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of 3,4,5-trichloropyridine (1 g, 5.45 mmol) in dichloromethane (20 mL) at 0° C., was added dropwise a 30% hydrogen peroxide solution (1.2 mL, 10.9 mmol). Following the addition, the temperature was allowed to rise to room temperature and was stirred for 15 hours. The reaction mixture was diluted with dichloromethane (50 mL) and was washed with water (10 mL) and then by brine (25 mL×2). The organic phase was dried (Na2SO4), concentrated under vacuum to afford the title product as a white solid (0.8 g, 74% yield). 1H NMR (400 MHz, d6-DMSO) δ: 8.78 (2H, s). MS m/z: 197.90 [M+H]+. the addition to rise to room temperature was washed with water (10 mL) The organic phase was dried (Na2SO4) concentrated under vacuum