Cesium carbonate → 6-{4-[4-(5-chloro-1H-indole-2-sulphonyl)-piperazine-1-carbonyl]-phenyl}-2-(2-dimethylamino-ethyl)-2H-pyridazin-3-one

関与物質

反応条件

反応手順

6-Chloro-2-(2-dimethylamino-ethyl)-2H-pyridazin-3-one (76 mg, 0.38 mmol), cesium carbonate (122 mg, 0.38 mmol) and bis(triphenylphosphine)palladium II chloride (21.9 mg, 0.03 mmol) was added to a microwave vial. The vial was evacuated and filled with argon twice. 4-({4-[(5-Chloro-1H-indol-2-yl)sulphonyl]piperazin-1-yl}carbonyl)phenyl boronic acid (140 mg, 0.31 mmol) dissolved in 4 mL 1,2-di-methoxyethane/water/ethanol (7:3:2) was added and the vial was once again evacuated and filled with argon. The reaction mixture was heated at 150° C. for 100 seconds, filtrated and purified by preparative HPLC using a gradient of acetonitrile/5% acetonitrile-water phase containing 0.1M ammonium acetate, to give 107 mg of 6-{4-[4-(5-chloro-1H-indole-2-sulphonyl)-piperazine-1-carbonyl]-phenyl}-2-(2-dimethylamino-ethyl)-2H-pyridazin-3-one after evaporation and freeze drying over night (60% yield).

情報源と証拠