反应详情

温度

65 °C

A mixture of 1-iodo-4-nitrobenzene (0.513 g, 2.06 mmol), 2-ethynyl pyridine (0.208 mL, 2.06 mmol), L-proline (47.4 mg, 0.412 mmol), Na2CO3 (43.7 mg, 0.412), NaN3 (0.1607 g, 2.47 mmol), (+)-sodium-L-ascorbate (40.8 mg, 0.206 mmol), copper (II) sulphate pentahydrate (16.4 mg, 0.103 mmol) in 9:1 DMSO-water (4 mL) is stirred in a stem-tube at 65° C. for 24 hours. After cooling, the reaction mixture is poured into ice-water (100 mL) and the resulting precipitate is collected by filtration, washed with 7% aq. NH3 and dried in vacuo to give the title compound as a brown solid (0.323 g, 59%). HPLC (254 nm) Rt 2.36 min (89%).

1. temperatureAfter cooling
2. filtrationthe resulting precipitate is collected by filtration
3. washwashed with 7% aq. NH3
4. customdried in vacuo