Acetic Acid → [1-amino(4-{[(R)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl](5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]-triazol-3-yl)methyl]amino}phenyl)methylene]carbamic acid 2-methylallyl ester

関与物質

反応手順

To a mixture of 4-{[(R)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl](5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]-triazol-3-yl)methyl]amino}benzamidine hydrochloride (5.0 g, 9.41 mmol), potassium carbonate (2.6 g, 18.8 mmol), and dimethyl sulfoxide (15 mL), carbonic acid 2-methylallyl ester phenyl ester [CAS No. 138621-73-5] (1.57 g, 8.19 mmol) was added, and the resulting mixture was stirred at room temperature for 4 days. Ethyl acetate (100 mL) and water (200 mL) were added to the reaction solution, and the aqueous layer was collected. Acetic acid (1.62 mL, 28.2 mmol) was added dropwise to the aqueous layer with stirring, and the precipitated solid was filtered and sequentially washed with water (20 mL) and diethyl ether (20 mL). The solid obtained was suspended in ethyl acetate, filtered, and then dried under air flow. The dried solid was suspended in ethyl acetate (50 mL), and the suspension was stirred for 1 day. The suspension was filtered, and the solid obtained was washed with ethyl acetate and dried under air flow to obtain the captioned compound (4.87 g) as a yellow solid.

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