反应详情

A mixture of Example 61B (0.1 g, 0.282 mmol), pyrrolidin-2-one (0.048 g, 0.565 mmol) cesium carbonate (0.130 g, 0.395 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.026 g, 0.028 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.025 g, 0.043 mmol) in DME (2 mL) was heated in a microwave (Personal Chemistry SmithSynthesizer) at 200° C. for 60 minutes. The mixture was filtered evaporated. The residue was purified by chromatography on silica gel with 20% to 80% ethyl acetate in hexane to provide the desired product. 1H NMR (500 MHz, DMSO-d6) δ ppm 2.01-2.08 (m, 2 H) 2.47 (t, J=8.09 Hz, 2 H) 3.81 (t, J=7.02 Hz, 2 H) 3.99 (s, 2 H) 5.67 (s, 1 H) 7.08 (d, J=7.63 Hz, 1 H) 7.30 (t, J=7.78 Hz, 1 H) 7.43-7.50 (m, 2 H) 7.66 (s, 1 H) 7.80-7.88 (m, 1 H) 8.04 (d, J=8.24 Hz, 1 H) 8.12 (d, J=7.93 Hz, 1 H).

1. filtrationThe mixture was filtered
2. customevaporated
3. customThe residue was purified by chromatography on silica gel with 20% to 80% ethyl acetate in hexane