反应详情

A solution of 3-bromo-5-nitropyridin-2-amine (655 mg, 3.0 mmol, 1.0 eq.) in 1:1 TEA/DMF (40 mL) was degassed with argon for 10 minutes, and ethynylbenzene (1.5 eq.), CuI (0.04 eq.), and PdCl2(PPh3)2 (0.04 eq.) were sequentially added. The mixture was degassed with argon for 10 minutes, and then stirred at room temperature for 16 hours. The volatiles were removed under reduced pressure, and CH2Cl2 (25 mL) was added. The mixture was sonicated for 15 minutes, cooled to 0° C., and collected by vacuum filtration to afford 5-nitro-3-(phenylethynyl)pyridin-2-amine (356 mg, 50%).

1. customThe mixture was degassed with argon for 10 minutes
2. customThe volatiles were removed under reduced pressure, and CH2Cl2 (25 mL)
3. additionwas added
4. customThe mixture was sonicated for 15 minutes
5. temperaturecooled to 0° C.
6. filtrationcollected by vacuum filtration