反应详情

温度

160 °C

A mixture of 1-(2-amino-4-chlorophenyl)-ethanone (1.85 g), copper powder (140 mg), KI (360 mg), K2CO3 (3.06 g) and iodobenzene (4.8 mL) in dibutyl ether (40 mL) was heated at 160° C. (oil bath temperature) overnight. More copper powder (140 mg), KI (360 mg), K2CO3 (3.06 g) and iodobenzene (4.8 mL) were added and the reaction mixture was heated at reflux overnight. The resulting mixture was then cooled and concentrated under reduced pressure. The residue was partitioned between water and ethyl acetate, the organic layer was separated and the aqueous layer was extracted with ethyl acetate (2×50 mL). The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The crude residue was purified by flash chromatography (EtOAc/hexane) to afford 2.2 g of 1-(4-chloro-2-phenylamino-phenyl)-ethanone.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux overnight
3. temperatureThe resulting mixture was then cooled
4. concentrationconcentrated under reduced pressure
5. customThe residue was partitioned between water and ethyl acetate
6. customthe organic layer was separated
7. extractionthe aqueous layer was extracted with ethyl acetate (2×50 mL)
8. washThe combined organic extracts were washed with brine
9. dry with materialdried over anhydrous sodium sulfate
10. filtrationfiltered
11. customevaporated under reduced pressure
12. customThe crude residue was purified by flash chromatography (EtOAc/hexane)