Phosphorus oxybromide → HCID 11345640, compound

Participants

Reaction Conditions

Reaction Steps

One hundred fifteen g. of 2-benzyl-6-ethoxypyridine and 200 g. of phosphorous oxybromide were heated together with stirring at 135°C. for 1 hour. The mixture gave off a gas during the first 15 minutes of the reaction but remained calm for the rest of the heating period. On cooling, the mixture became an intractable tar and the reaction flask was broken to obtain the crude product. It was partitioned between 2 liters of water, 270 ml. of 10N sodium hydroxide solution and 1 liter of chloroform. The organic extract was washed with 1 liter of water and dried over magnesium sulfate. Removal of the desiccant and solvent yielded a dark oil which was extracted with 750 ml. of petroleum ether (b.p. 60°-80°C.), and treated with decolorizing charcoal. Removal of the solids and solvent yielded the product as an amber oil. This material was used without further purification for the next step.

Provenance & Evidence