反应详情

温度

100 °C

A 250 mL round bottom flask flushed with N2 was charged with 2-chloro-5-iodo-pyridin-4-ylamine (1.00 g, 3.93 mmol), 5-ethynyl-nicotinic acid methyl ester (0.633 g, 3.93 mmol), copper(I) iodide (0.037 g, 0.196 mmol), bis(triphenylphosphine)palladium(II) chloride (0.138 g, 0.196 mmol) and triethyl amine (50 mL). The reaction mixture was stirred at 100° C. for 3 h. The reaction was cooled to room temperature, filtered and the precipitate washed thoroughly with ethyl acetate. The filtrate was washed with water twice. The organic layer was dried over sodium sulfate and concentrated in vacuo to afford crude product 5-(4-amino-6-chloro-pyridin-3-ylethynyl)-nicotinic acid methyl ester as a brown solid which was taken onto next step without any purification. ESI-MS: m/z 288.0 (M+H)+

1. customA 250 mL round bottom flask flushed with N2
2. temperatureThe reaction was cooled to room temperature
3. filtrationfiltered
4. washthe precipitate washed thoroughly with ethyl acetate
5. washThe filtrate was washed with water twice
6. dry with materialThe organic layer was dried over sodium sulfate
7. concentrationconcentrated in vacuo