反应详情

温度

85 °C

To a solution of 2,5-dichlorobenzonitrile (10 g, 58.1 mmol) in DMF (100 ml) was added cesium carbonate (22.7 g, 69.8 mmol) and 1,2,4-triazole (4.8 g, 69.8 mmol) and the reaction mixture was stirred at 65° C. for 5.5 h, at 75° C. for 16 h, at 85° C. for 7 h. More 1,2,4-triazole (5 g) was added and the reaction mixture was stirred at 85° C. for 18 h and at 100° C. for 4 h. After cooling to room temperature, the mixture was diluted with water and extracted with EtOAc 3 times. The combined organic layer was washed with aqueous LiCl, dried on sodium sulfate, concentrated in vacuo to give 5-chloro-2-[1,2,4]triazol-1-yl-benzonitrile as a white solid which was used in the next step without further purification.

1. stirringthe reaction mixture was stirred at 85° C. for 18 h and at 100° C. for 4 h
2. temperatureAfter cooling to room temperature
3. extractionextracted with EtOAc 3 times
4. washThe combined organic layer was washed with aqueous LiCl
5. customdried on sodium sulfate
6. concentrationconcentrated in vacuo