2-Methylmorpholine → HCID 13292750, compound

Participants

Reaction Steps

8.00 mg. of 1,4-dichloro-8-methyl-7-phenylpyrido[3,4-d]pyridazine was heated together with 2 g. of 2-methyl-morpholine at 120° C for 1.5 hours, after which time the excess 2-methylmorpholine was distilled off. To the residue was added 30 ml. of water and the resultant crystals were recovered by filtration and purified by column chromatography (silica gel; acetone: benzene=1:8) in the same manner described in Example 3. After removal of the solvent, the residue was dissolved in 20 ml. of ethanol. Following the addition of 2 ml. of water, the solution was concentrated to dryness. To the residue was added 20 ml. of water, followed by stirring. The resultant crystals were dried in a vacuum dryer at 50°-60° C for 12 hours, whereupon 600 mg. of 8-methyl-1,4-bis(2-methylmorpholino)-7-phenylpyrido-[3,4-d]pyridazine was obtained. Melting point: 96°-99° C.

Provenance & Evidence