O1[CH:5]2[C:6]3[C:7]4[C:12]([C:13]5[C:18]([C:19]=3[CH:2]1[CH:3]=[CH:4]2)=[CH:17][CH:16]=[CH:15][CH:14]=5)=[CH:11][CH:10]=[CH:9][CH:8]=4.[Br:20][C:21]1[CH:26]=[CH:25][C:24](I)=[CH:23][CH:22]=1.BrC1C=CC=C(I)C=1.C(N(CC)CC)C>[Zn].Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1(C)C=CC=CC=1>[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:15]2[CH:16]=[CH:17][C:18]3[C:19]4[C:6](=[CH:5][CH:4]=[CH:3][CH:2]=4)[C:7]4[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=4)[C:13]=3[CH:14]=2)=[CH:23][CH:22]=1Compound A (4.0 g, 16.4 mmol), zinc (10.72 g, 163.9 mmol), PdCl2(PPh3)2 (1.16 g, 1.7 mmol), and 1-bromo-4-iodobenzene (4.64 g, 16.4 mmol) or 1-bromo-3-iodobenzene were charged in a two-necked bottle. The bottle was then vacuumed and purged with nitrogen, and dried toluene (100 mL) and triethyl amine (23.0 mL, 165.9 mmol) were added to the bottle. The mixture in the bottle was heated to 110° C. for reaction for 24 hours, and the resulting was filtered to remove metal. The filtrate was condensed to remove the solvent, and then purified by chromatography with hexanes to obtain B (3.90 g, yield=62%) as white solid.
Wird geladen…