Water → HCID 86600907, compound

Participants

Reaction Steps

A solution of 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarbonitrile 4-oxide (1.54 g) in DMF (30 ml) was stirred at 0° C. Phosphorous oxychloride (1.58 ml) was dropped to the solution and the reaction mixture was stirred under same condition for 3 hours. Water was added to the reaction mixture. The reaction mixture was stirred at 20° C. for 20 hours to give a yellow precipitate. The precipitate was collected by filtration to obtain yellow powder. The residue was purified by silica gel column chromatography eluted with a mixture of n-hexane and EtOAc. The fractions were concentrated in vacuo to obtain N′-[6-chloro-3-cyano-5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinyl]-N,N-dimethylimidoformamide (1.0 g) as white powder.

Provenance & Evidence