反应详情

温度

165 °C

To a reaction vessel containing a re-purified solution of 5-bromo-3,7-dimethyl-1H-indazole (prepared as described for Acid Preparation 26, 285 mg, 1.27 mmol) in dioxane (1.3 mL) was added hexacarbonylmolybdenum (264 mg, 1.0 mmol), Herrmann's catalyst (93 mg, 0.1 mmol) and a solution of Na2CO3 in water (636 mg in 2 mL water). The suspension was heated in a microwave at 165° C. for 15 minutes (high absorption). The vial was vented, acidified with 1 N HCl (to pH 2). The reaction mixture was filtered through diatomaceous earth, washed with EtOAc and the organic layer was washed with saturated aqueous NaCl (3×). The organic extract was concentrated to yield the title compound as a pink solid (65 mg, 17%).

1. custom(high absorption)
2. filtrationThe reaction mixture was filtered through diatomaceous earth
3. washwashed with EtOAc
4. washthe organic layer was washed with saturated aqueous NaCl (3×)
5. extractionThe organic extract
6. concentrationwas concentrated