Methyl iodide → HCID 58938671, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-mesityl-4-(propylamino)-1,6-dihydro-7H-pyrrolo[2,3-d]pyridazin-7-one (29.8 mg, 0.092 mmol), methyl iodide (0.011 ml, 0.18 mmol), potassium carbonate (25.4 mg, 0.18 mmol) and DMF (1 ml) was stirred at 60° C. for 4 hours. The mixture was diluted with water (30 ml) and extracted with ethyl acetate (30 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. A mixture of the residue, methyl iodide (0.1 ml), sodium hydride (60% in oil, 8 mg, 0.2 mmol) and DMF (2 ml) was stirred room temperature for 3 hours. The mixture was diluted with water (30 ml) and extracted with ethyl acetate (30 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with hexane/ethyl acetate (10:1-5:1) to give 6.5 mg (20%) of the title compound as crystals.

Provenance & Evidence