Phosphorus oxybromide → HCID 59234241, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of intermediate 4 (39 g, 203 mmol) in DMF (600 ml) was added phosphoric tribromide (116 g, 406 mmol) and the mixture was heated at 110° C. for 1.5 hours. After cooling in an ice bath the solution was partitioned between water and EtOAc. After three extractions with EtOAc the combined organic fractions were washed with brine, dried over Na2SO4 and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; DCM as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 6 (36.7 g, 72%).

Provenance & Evidence