反应详情

A suspension of pyridin-3-amine (5.08 mg, 0.054 mmol), 6-fluoro-3-[4-(4-iodo-3-methoxyphenyl)-1H-1,2,3-triazol-1-yl]-1-(2,2,2-trifluoroethyl)-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one (30 mg, 0.054 mmol), potassium carbonate (8.14 mg, 0.059 mmol), X-Phos (12.76 mg, 0.027 mmol), and tris(dibenzylideneacetone)dipalladium (9.81 mg, 0.011 mmol) were combined in a μwave vial and dissolved in t-amyl alcohol (1071 μl). The reaction was microwaved at 130° C. for 20 min. The reaction mixture was filtered, and the solvent was removed in vacuo. Analytically pure material was obtained by purification by preparative HPLC Reverse phase (C-18), eluting with acetonitrile/water+0.05% Formic Acid. Lyophilisation afforded 6-fluoro-3-{4-[3-methoxy-4-(pyridin-3-ylamino)phenyl]-1H-1,2,3-triazol-1-yl}-1-(2,2,2-trifluoroethyl)-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one

1. customThe reaction was microwaved at 130° C. for 20 min
2. filtrationThe reaction mixture was filtered
3. customthe solvent was removed in vacuo
4. customAnalytically pure material was obtained by purification by preparative HPLC Reverse phase (C-18)
5. washeluting with acetonitrile/water+0.05% Formic Acid