1,3,5-Trimethoxy-4-iodobenzene → 1,3,5-Trimethoxy-2-(2,4,6-trimethoxyphenyl)benzene
반응식
I[C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[CH:4][C:3]=1[O:12][CH3:13]>[Cu]>[CH3:13][O:12][C:3]1[CH:4]=[C:5]([O:10][CH3:11])[CH:6]=[C:7]([O:8][CH3:9])[C:2]=1[C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[CH:4][C:3]=1[O:12][CH3:13]참가 물질
3
반응 조건
- 온도
- 235 °C
실험 절차
Compound 6 (7.0 g, 0.024 mol) and copper powder (2.0 g, 0.03 1 mol) were mixed thoroughly and transferred to a heavy wall, pressure vessel. The vessel was placed into a sand-bath at the initial temperature of 120° C. Once the vessel was secured, the temperature of the bath was raised to 235° C. in 15 min and kept at 235° C. for 1 h. The vessel was allowed to cool and the contents removed and powdered. The product was extracted with methanol for 18 h in a soxhlet. The resultant solution was concentrated in vacuo. Purification of the crude reaction mixture via column chromatography (1:5 ethyl acetate/hexane) yielded 7 (3.1 g, 78%) as a white solid.