反应 #3229365
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07261952B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 60 g of 2,5-Dibromo-p-xylene (0.227 mole), 42.4 g of CuCN (0.568 mole) and 300 ml of dimethylformamide were added into a round-bottom flask, and then the reaction was performed at 130° C. for 12 hours. After completion of the reaction, the reaction mixture was added to the mixing solution of 300 ml of water and 300 ml of aqueous ammonia, and extracted crystal therefrom was filtered. Then, the crystal was added again to the mixing solution of 100 ml of water and 300 ml of aqueous ammonia, mixed and filtered. The obtained crystal was added to 2,000 ml of toluene, heated to dissolve, and treated with active carbon. The filtrate was evaporated in vacuum, and then 300 ml of hexane was added thereto to obtain 20 g of white crystal (0.128 mole, yield: 56%). After completion of the reaction extracted crystal therefrom was filtered Then, the crystal was added again to the mixing solution of 100 ml of water and 300 ml of aqueous ammonia mixed filtered The obtained crystal was added to 2,000 ml of toluene heated to dissolve treated with active carbon The filtrate was evaporated in vacuum 300 ml of hexane was added
来源 ID: ord-beae829bb0074c1b9c7451dcc976c558