反应详情

A suspension of 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 (50 mg, 0.089 mmol), 18-CROWN-6 (28.3 mg, 0.107 mmol), pyridin-4-amine (9.24 mg, 0.098 mmol), BINAP (11.11 mg, 0.018 mmol), sodium tert-butoxide (17.15 mg, 0.178 mmol), and tris(dibenzylideneacetone)dipalladium (4.09 mg, 4.46 μmol) were combined in a microwave vial and dissolved in THF (892 μl). The reaction was irradiated in the microwave at 160° C. for 15 minutes. 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-4-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 irradiated in the microwave at 160° C. for 15 minutes
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