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ChemicalBook CAS DataBase List 2,8-DIBROMODIBENZOFURAN

2,8-DIBROMODIBENZOFURAN synthesis

10synthesis methods
-

Yield:10016-52-1 87%

Reaction Conditions:

with bromine in acetic acid at 120; for 6 h;Inert atmosphere;

Steps:

4.3. Synthesis and characterizations of L2
To a round bottom flask, Diphenylene-oxide (8.40 g, 50 mmol), bromine (2.6 mL) dissolved in 30 mL glacial acetic acid were added. The resultant suspension was heating for 6 h under nitrogen at 120 C. After cooling to 25 C, the intermediate product 2 was recovered by filtration and recrystallization in acetic acid and vacuum drying as a white solid (12.2 g, 75%). 1H NMR (400 MHz,CDCl3) d (ppm): 8.03 (s, 2H), 7.58 (d, J 8.0 Hz, 2H), 7.44 (d, J 8 Hz,2H) (Fig. S27) [46]. To a solution of 2 (0.324 g, 1.0 mmol) and 4-([2,2': 6', 2''- terpyridyl]-4'-) - benzene boric acid (0.88 g,2.50 mmol) in THF (100 mL), aqueous NaOH (160 mg, 4.0 mmol) was added. The mixture was degassed for 10 min, then Pd(PPh3)4(115 mg, 0.10 mmol) was added. Following the procedure L1, thepure product L2was obtained as a white solid (0.55 g, 70%).

References:

Liu, Qianqian;Yang, Xiaoyu;Wang, Meng;Liu, Die;Chen, Mingzhao;Wu, Tun;Jiang, Zhiyuan;Wang, Pingshan [Tetrahedron,2019,vol. 75,# 16,p. 2400 - 2405] Location in patent:supporting information

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