Potassium Phosphate, Tribasic → HCID 86712983, compound

Participants

Reaction Conditions

Reaction Steps

The compound (600 mg, 1.05 mmol) obtained in Example 89-1), 3-chloro-6-methylpyridazine (161 mg, 1.26 mmol), tris(dibenzylideneacetone)dipalladium (96 mg, 0.10 mmol), tricyclohexylphosphine (29 mg, 0.10 mmol), and tripotassium phosphate (458 mg, 2.09 mmol) were dissolved in a mixed solvent of 1,4-dioxane (2 mL) and water (1 mL), and the mixture was stirred at 140° C. for 2 h under microwave irradiation. The reaction mixture was cooled to room temperature, then diluted with methylene chloride (200 mL), and separated into organic and aqueous layers by the addition of saturated aqueous sodium hydrogencarbonate. The organic layer was washed with saturated sodium chloride solution and then dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography (methanol:ethyl acetate=0:100 to 20:80) to obtain the title compound (366 mg, 65%) as a brown solid.

Provenance & Evidence