4,6-Dimethylpyrimidin-2-ol → 2-[5-chloro-4-(4,6-dimethyl-pyrimidin-2-yloxy)-6-oxo-6H-pyridazin-1-yl]-3-cyclopentyl-propionic acid methyl ester

関与物質

反応条件

反応手順

A solution of 3-cyclopentyl-2-(4,5-dichloro-6-oxo-6H-pyridazin-1-yl)-propionic acid methyl ester (Intermediate 79 step 1, 15.4 g, 48 mmol) in N,N-dimethylformamide (150 mL) was treated with 4,6-dimethyl-pyrimidin-2-ol (5.98 g, 48 mmol) and potassium carbonate (8 g, 58 mmol). The reaction was heated at reflux for 12 h. At this time, the reaction was cooled to 25° C. and concentrated in vacuo. The residue was partitioned between water and methylene chloride. The aqueous layer was back extracted with methylene chloride. The combined organics were washed with a saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated in vacuo. Chromatography (5/1 petroleum ether/ethyl acetat) afforded 2-[5-chloro-4-(4,6-dimethyl-pyrimidin-2-yloxy)-6-oxo-6H-pyridazin-1-yl]-3-cyclopentyl-propionic acid methyl ester (7.47 g, 38%).

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