反应详情

温度

125 °C

To a degassed solution of methyl 7-ethyl-3-iodo-1H-indazole-5-carboxylic acid (100 mg, 0.30 mmol) in DME (2.5 mL) was added degassed boroxine solution (50%, 0.28 mL) followed by palladium tetrakistriphenylphosphine (3.5 mg, 0.003 mmol) and 2 M Na2CO3 (0.57 mL). The mixture was heated in a microwave reactor (very high absorption setting) at 125° C. for 10 minutes and then at 165° C. for 10 minutes. The reaction was extracted with EtOAc and washed with saturated aqueous NaCl. The organic extract was reduced and the crude material was purified by silica gel chromatography (40 g column) using 0-40% EtOAc/heptane to afford methyl 7-ethyl-3-methyl-1H-indazole-5-carboxylic acid (18 mg, 27%).

1. customdegassed boroxine solution (50%, 0.28 mL)
2. extractionThe reaction was extracted with EtOAc
3. washwashed with saturated aqueous NaCl
4. extractionThe organic extract
5. customthe crude material was purified by silica gel chromatography (40 g column)