Reaktion #1279224

Reaktionsgleichung

3,4,5-trichloropyridine

hydrogen peroxide

→

title product

Ausbeute 74.0%

3,4,5-trichloro-1-oxido-pyridin-1-ium

Ausbeute 74.0%

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONthe addition
2. 2
   Sonstigeto rise to room temperature
3. 3
   Waschenwas washed with water (10 mL)
4. 4
   TrocknenThe organic phase was dried (Na2SO4)
5. 5
   Einengenconcentrated under vacuum

Vorschrift

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]+.

Quelle