反应详情

A solution of iodine monochloride (32.5 g, 200 mmol) in acetic acid (120 mL) was added portionwise over 2 h to a mixture of 6-bromo-9H-dipyrido[2,3-b;4′,3′-d]pyrrole (5.0 g, 20 mmol) and sodium acetate (18.2 g, 221 mmol) in acetic acid (120 mL) at 100° C. The reaction mixture was cooled to ambient temperature and poured into saturated sodium metabisulfite solution (20% w/w, 400 mL). The resultant precipitate was collected by filtration and the solid was washed with water (50 mL) and diethyl ether (2×50 mL) then dried at 45° C. until constant weight was achieved, to afford the title compound as a grey solid (6.3 g, 83%). 1H NMR (DMSO-D6, 300 MHz) 12.49 (s, 1H); 9.14 (d, J=2.1 Hz, 1H); 8.79 (d, J=2.1 Hz, 1H); 8.71 (s, 1H); 8.49 (s, 1H). LCMS (Method B): RT=3.40 min, M+H+=374/376.

1. filtrationThe resultant precipitate was collected by filtration
2. washthe solid was washed with water (50 mL) and diethyl ether (2×50 mL)
3. customthen dried at 45° C. until constant weight