反应详情

温度

50 °C

A mixture of Example 61a (0.130 g, 0.322 mmol), methanesulfonamide (0.046 g, 0.482 mmol), cesium carbonate (0.136 g, 0.418 mmol), palladium acetate (3.61 mg, 0.016 mmol), and Xantphos (0.014 g, 0.024 mmol) in dioxane (3 mL) and DMF (0.1 mL) was heated at 160° C. for 30 minutes in a Biotage microwave reactor. The mixture was concentrated. The residue was treated with EtOAc and washed with 20% brine. The emulsion of the organic layer was concentrated. The solid was suspended in dioxane (4 mL), treated with 20% sodium hydroxide (0.15 mL, 0.322 mmol), and heated at 50° C. for 3 hours. The reaction mixture was concentrated. The residue was treated with DMSO/MeOH and purified by reverse-phase HPLC as described in Example 56 to give the title compound (6.0 mg) as trifluoroacetic acid salts. 1H NMR (300 MHz, DMSO-d6) ppm 3.36 (s, 3H), 7.26 (dd, J=7.93, 4.76 Hz, 1H), 7.41 (d, J=0.79 Hz, 1H), 7.55 (d, J=1.19 Hz, 1H), 8.27-8.40 (m, 3H), 10.76 (s, 1H), 12.36 (s, 1H). MS (ESI+) m/z 322.8 (M+H)+.

1. concentrationThe mixture was concentrated
2. additionThe residue was treated with EtOAc
3. washwashed with 20% brine
4. concentrationThe emulsion of the organic layer was concentrated
5. concentrationThe reaction mixture was concentrated
6. additionThe residue was treated with DMSO/MeOH
7. custompurified by reverse-phase HPLC