3-Aminopyridine → (2R)-2-amino-N-{5-(4,4-dimethyl-2,5-dioxo-3-{[2-(pyridin-3-ylamino)pyridin-4-yl]methyl}imidazolidin-1-yl)-2-[(trifluoromethyl)thio]phenyl}-2-phenylacetamide

関与物質

反応条件

反応手順

To a solution of 33 mg of (2R)—N-(5-{3-[(2-chloropyridin-4-yl)methyl]-4,4-dimethyl-2,5-dioxoimidazolidin-1-yl}-2-[(trifluoromethyl)thio]phenyl)-2-[(9H-fluoren-9-ylacetyl)-amino]-2-phenylacetamide obtained in stage e) below in 1 mL of dioxane are successively added, under argon, 14 mg of 3-aminopyridine, 3 mg of (9,9-dimethyl-9H-xanthene-3,6-diyl)bis(diphenylphosphine) (Xantphos), 1.1 mg of palladium acetate and 61 mg of caesium carbonate. The reaction mixture is heated at 110° C. for 3 h, filtered and washed with twice 10 mL of dioxane, and the filtrate is then concentrated under reduced pressure. The residue is purified by HPLC (gradient: water/acetonitrile containing 0.1% formic acid) to give 5 mg of (2R)-2-amino-N-{5-(4,4-dimethyl-2,5-dioxo-3-{[2-(pyridin-3-ylamino)pyridin-4-yl]methyl}imidazolidin-1-yl)-2-[(trifluoromethyl)thio]phenyl}-2-phenylacetamide, the characteristics of which are as follows:

情報源と証拠