Hydrogen Peroxide → HCID 178488303, compound

Participants

Reaction Steps

45 ml of hydrogen peroxide (15% strength) are added dropwise to a stirred solution of 152.5 mmol of 3-methoxypyridin-2-ol [20928-63-6] in 152 ml of hydrobromic acid (48% strength) at 70° C. over the course of one hour so that the temperature remains at 70° C. The mixture is stirred at this temperature for a further hour. It is then cooled to room temperature, and 1M sodium thiosulphate solution is added to the reaction solution until excess bromine is completely reduced (decolorization). Saturated sodium carbonate solution is then added to the resulting solution until the pH is 4. A solid precipitates and is filtered off. Further saturated sodium carbonate solution is added to the clear filtrate until the pH reaches 11. It is extracted with dichloromethane (3×), and the combined organic phases are dried with sodium sulphate and evaporated. The title compound is identified by means of the Rf from the residue by flash chromatography (SiO2 60 F).

Provenance & Evidence