Potassium Acetate → HCID 10714321, compound

Participants

Reaction Steps

Potassium acetate (380 mg) and acetic acid (6 ml) were added to (-)-(3S,4R)-4-[(6-chloro-3-pyridazinyl)amino]-6-cyano-3,4-dihydro-2,2-bis(methoxymethyl)-2H-1benzopyran-3-ol (750 mg) obtained in Example 5, and the mixture was refluxed with stirring for 5 hours. The reaction mixture was filtered and the residue was washed with acetic acid. The residue obtained by removing the solvent from the filtrate under reduced pressure was purified by silica gel column chromatography (ethyl acetate:ethanol=95:5), whereby (-)-(3S,4R)-4-[(6-acetyloxy-3-pyridazinyl)amino]-6-cyano-3,4-dihydro-2,2-bis(methoxymethyl)-2H-1-benzopyran-3-ol (180 mg, 22.6%) and (-)-(3S,4R)-6-cyano-3,4-dihydro-4-[(1,6-dihydro-6-oxo-3-pyridazinyl)amino]-2,2-bis(methoxymethyl)-2H-1-benzopyran-3-ol (500 mg, 69.9%) were obtained in the order of elution.

Provenance & Evidence