反应详情

温度

150 °C

To a solution of 1.5 g (5.6 mmol) of 6-amino-5-bromo-1H-indazole-7-carboxylic acid methyl ester, prepared as in step a in example 16, in 3 mL of N,N-dimethylformamide under an atmosphere of argon is added 785 μL (5.6 mmol) of trimethylsilylacetylene, 8.65 mL of diethylamine (83.2 mmol), 194 mg (0.28 mmol) of dichlorobis(triphenylphosphine)palladium II and 53 mg (0.28 mmol) of copper iodide. The reaction mixture is stirred in a microwave oven at 150° C. for 5 minutes, filtrated over Celite (washing with ethyl actetate) and concentrated in vacuo. The residue is purified by flash chromatography (SiO2, hexane/ethyl acetate 2:1) to afford 970 mg of the product (61%) as a yellowish solid; LC/MS:288/289 (M+H)+.

1. filtrationfiltrated over Celite (washing with ethyl actetate)
2. concentrationconcentrated in vacuo
3. customThe residue is purified by flash chromatography (SiO2, hexane/ethyl acetate 2:1)