Abstract A new synthesis of 7-bromo-1, 3-dihydro-3-hydroxy-5-(2′-pyridyl)-2H-1, 4- benzodiazepin-2-one (5) is described. Starting from bromazepam (3), C (3) acylation with lead tetraacetate/potassium iodide in acetic acid affords 4, while its mild hydrolysis according to our recently described method (5) gives 5. Improved hexamine cyclization of 1 into 3, via quaternary hexaminium salt 2, is discussed, and identification of the ...