反应详情

温度

80 °C

A mixture of 3-bromopyridine-2-carbonitrile (150 mg, 0.98 mmol), 3-tert-butyl-1-methyl-1H-pyrazol-5-amine (179 mg, 0.98 mmol), cesium carbonate (638 mg, 1.96 mmol), BINAP (98 mg, 0.16 mmol) and Pd2(dba)3 (90 mg, 0.10 mmol) was taken in anhydrous toluene (2 mL) and heated to 80° C. for 24 h under nitrogen atmosphere. The reaction mixture was cooled to rt, diluted with ethyl acetate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography using EtOAc/Hex (1:9 to 1:4, v/v) as the eluent. The product was obtained as a yellow oil (145 mg, 58%). ES-MS m/z 256.1 (MH+); HPLC RT (min) 2.37.

1. temperatureThe reaction mixture was cooled to rt
2. filtrationfiltered
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by silica gel chromatography