反应详情

温度

180 °C

Pre-treatment of copper powder: The copper powder (5.0 g, 78 mmol) was weighted and added into to a 20 mL of 2% iodine/acetone solution. The mixture was stirred for 10 minutes, and filtered in vacuum. The resultant was added into 20 mL of mixed solution of acetone:hydrochloric acid=1:1. The resultant mixture was stirred for 10 minutes, filtered, and dried in vacuum. The 2,6-dinitrochlorobenzene (3.04 g, 15 mmol) and copper powder (2.88 g, 45 mmol) were added into a 250 mL round flask, and were mixed homogeneously. Under the protection of nitrogen gas, the mixture was heated at 180° C. under stirring in an oil bath for two hours. Upon completion of the reaction, the solid in the flask was grounded, and dissolved in 20 mL of ethyl acetate. The solid was filtered off, and the filtration was collected and rotary evaporated. The residue was recrystallized from a mixed solution of ethyl acetate: petroleum ether=10:1, to precipitate a pale yellow needle-like crystal. The crystal was filtered in vacuum, to afford the product in a yield of 63.9%.

1. filtrationfiltered in vacuum
2. additionThe resultant was added into 20 mL of mixed solution of acetone
3. stirringThe resultant mixture was stirred for 10 minutes
4. filtrationfiltered
5. customdried in vacuum
6. additionwere mixed homogeneously
7. stirringunder stirring in an oil bath for two hours
8. customUpon completion of the reaction
9. filtrationThe solid was filtered off
10. filtrationthe filtration
11. customwas collected
12. customThe residue was recrystallized from a mixed solution of ethyl acetate
13. custompetroleum ether=10:1, to precipitate a pale yellow needle-like crystal
14. filtrationThe crystal was filtered in vacuum
15. customto afford the product in a yield of 63.9%