Peracetic Acid → HCID 86706667, compound

Participants

Reaction Steps

Under stirring, 205 ml (1.2 mol) peracetic acid (39% solution in acetic acid) was added to a solution of 98.8 g (0.60 mol) 1-chloro-[2,6]naphthyridine in 500 ml ethyl acetate and the mixture was stirred 18 hours at room temperature. The reaction mixture was diluted with water and acetic acid, treated with portions of sodium disulfite under stirring until a peroxide test was negative. Then the mixture was adjusted to pH value of 8 with aqueous NaOH. The solids were filtered off, washed with water and dried yielding 1-chloro-[2,6]-naphthyridine 6-oxide as slightly yellow crystals. The organic phase of the filtrate was separated, dried over sodium sulfate and evaporated. The residue was crystallized from tert-butyl-methyl-ether yielding another crop of product. HPLC/MS (A): 1.16 min, [M+H] 181.

Provenance & Evidence