反应详情

To toluene 3.0 mL solution of methyl 2-(4-fluoroanilino)-4-iodobenzoate 0.30 g, allylbenzene 0.16 mL and triethylamine 0.11 mL was added palladium acetate 9 mg, and it was heated and refluxed under nitrogen atmosphere for 2 hours. After the reaction mixture was cooled to room temperature, palladium acetate 18 mg was added to it, and it was heated and refluxed under nitrogen atmosphere for 2 hours. After the reaction mixture was cooled to room temperature, palladium acetate 18 mg was added, and it was heated and refluxed under nitrogen atmosphere for 1 hour. After the reaction mixture was cooled to room temperature, palladium acetate 18 mg was added, and it was heated and refluxed for 2 hours. After the reaction mixture was cooled to room temperature, insoluble matter was filtrated, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [eluent; hexane:ethyl acetate=20:1] to give methyl 2-(4-fluoroanilino)-4-(3-phenyl-1-propenyl)benzoate.

1. temperaturewas heated
2. temperaturerefluxed under nitrogen atmosphere for 2 hours
3. temperaturewas heated
4. temperaturerefluxed under nitrogen atmosphere for 2 hours
5. temperatureAfter the reaction mixture was cooled to room temperature
6. temperatureit was heated
7. temperaturerefluxed under nitrogen atmosphere for 1 hour
8. temperatureAfter the reaction mixture was cooled to room temperature
9. temperatureit was heated
10. temperaturerefluxed for 2 hours
11. temperatureAfter the reaction mixture was cooled to room temperature
12. filtrationinsoluble matter was filtrated
13. customthe solvent was removed under reduced pressure