反应详情

温度

80 °C

A mixture of 3-bromo-5-nitro-1-trityl-1H-indazole (4.83 g, 10 mmol), ethynyl-trimethyl-silane (1 g, 10 mmol), copper (I) iodide (91 mg, 0.5 mmol), PdCl2(dppf) (337 mg, 0.5 mmol) and triethylamine (1.2 g, 12 mmol) in DMF (50 mL) was stirred overnight at 80° C. under argon. Then ethyl acetate (100 mL) was added, followed by water. The organic layer was collected and aqueous layer was extracted three times with ethyl acetate. The combined organic fraction was washed with water and then brine. The solvent was removed under vacuum and the product was purified using chromatography (20% hexane in dichloromethane) to give desired product (3.4 g) in 67% yield.

1. customThe organic layer was collected
2. extractionaqueous layer was extracted three times with ethyl acetate
3. washThe combined organic fraction was washed with water
4. customThe solvent was removed under vacuum
5. customthe product was purified