Phosphorus tribromide → HCID 22022774, compound

Participants

Reaction Steps

g (0.002 moles) of the product (X), obtained according to the preparation reported in the preceeding example 5, are heated with 10 ml (0.105 moles) of PBr3 to 110° C. for 40 minutes. The reaction mass is hydrolyzed in ice, extracted with ethyl ether, the ether extract is washed with an aqueous solution of NaHCO3 (10%), dried on Na2SO4, filtered and the ether solution is dried. The residue is dissolved in 20 ml of acetic acid and 1 g of Zn in powder form is added. The mixture is stirred for 1 h at room temperature, hydrolyzed in water and then extracted with ethyl ether. The ether extract is neutralized with an aqueous solution of NaHCO3 (10%), dried with Na2SO4, filtered and dried. The residue is purified on a silica gel column (eluant petroleum ether) obtaining, after evaporation of the pure fractions, 0.8 g of pure product (yield 76.6%).

Provenance & Evidence