With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.17217-57-1,4,4′-Dimethoxy-2,2′-bipyridine,as a common compound, the synthetic route is as follows.
4,4?-Dimethoxy-2, 2?-bipyridine (188 mg, 0.87 mmol) and sodium hexafluorophosphate (146 mg, 0.87 mmol) added to a suspension of 6 (200 mg, 0.17 mmol) in chloroform (40 mL). The mixture was refluxedat 60 ¡ãC for 48 h. The solution was concentrated to approximately 2 mLunder vacuum. Ether (20 mL) was added to the solution to give a yellow precipitate. After filtration, the crude product was purified by column chromatography (alumina gel; eluted with dicloromethane/methanol, 100:1 v/v) to give a yellow solid 3 (146 mg, 69percent). 1H NMR (400 MHz,CD3CN): delta=9.7 (d, 3JPH=20 Hz, 1 H, IrCH), 7.7?8.7 (m, 6 H, bipyridyl),7.0?7.7 (m, 30 H, PPh3), 5.2?6.4 (m, 4 H, phenyl), 4.04, 4.00 (s,6H, OCH3). 31P NMR (162 MHz, CD3CN): delta=11.5 (d, J=9.2 Hz,CPPh3), – 9.9 (s, IrPPh3). 13C NMR (101 MHz, CD3CN): delta=193.7 (s,IrCH), 167.7 (d, 2JPC=23.9 Hz, COCH3), 157.6, 157.3, 153.9, 150.9 (s,bipyridyl), 152.5 (d, 2JPC=19.4 Hz, IrCHC(PPh3)C), 146.3 (d, 2JPC=19.1 Hz, IrC), 112.1?136.1 (m, PPh3, phenyl, and bipyridyl),110.7 (d, 1JPC=90.6 Hz, IrCHC(PPh3)), 54.6, 54.3 ppm (s, OCH3). HRMS:m/z [M]+ calcd for C56H47ClIrN2O2P2+ 1069.2425, found1069.2422. IR (KBr, cm?1): 840 (P?F). Anal. Calcd for C56H47ClF6IrN2O2P3: C 55.38, H 3.90, N 2.31. Found: C 55.09, H 4.11,N 2.55percent.
17217-57-1, 17217-57-1 4,4′-Dimethoxy-2,2′-bipyridine 2733927, acatalyst-ligand compound, is more and more widely used in various fields.
Reference£º
Article; Hu, Yuxuan; Dong, Yubao; Sun, Xiaona; Zuo, Guorui; Yin, Jun; Liu, Sheng Hua; Dyes and Pigments; vol. 156; (2018); p. 260 – 266;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI