Phosphorus tribromide → 4-broMo-5-Methoxy-2-Methylpyridine

Participants

Reaction Steps

To a solution of 4-bromo-5-methoxy-2-methyl-pyridine 1-oxide (Step AL4) (150 mg, 0.7 mmol) in CHCl3 (2 mL) at 10° C. was added dropwise PBr3 (78 μL, 0.826 mmol). The mixture was stirred at rt for 4 h, then at 50° C. for 1 h. The reaction mixture was dissolved in CH2Cl2 and extracted with a saturated aqueous solution of NaHCO3, washed with brine, dried (Na2SO4), filtered and concentrated. The product was crystallised (CH2Cl2/TBME). ESI-MS: tR=0.69 min, [M+H]+ 202.0/204.0 (LC-MS 1).

Provenance & Evidence