With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.103946-54-9,4′-Methyl-[2,2′-bipyridine]-4-carboxylic acid,as a common compound, the synthetic route is as follows.
bpyAc (34.9 mg, 0.163 mmol) and fac-[Re(CO)3(dmso-O)3](PF6)(102.8 mg, 0.157 mmol) were dissolved in dry acetone (10 mL).The mixture was stirred at reflux for 4 h under argon. The solutionwas concentrated at ca. 2 mL and the precipitation of the productwas induced by slow diffusion of diethyl ether. A pure yellowpowder was isolated by filtration and washed with ether. Yield83 mg, 0.117 mmol (75%). Anal. Calc. for C17H16F6N2O6PReS(Mw = 707.56): C, 28.86; H, 2.28; N, 3.96; S, 4.53. Found: C,28.97; H, 2.35; N, 3.78; S, 4.62%. 1H NMR (d, 500 MHz, CD3NO2):9.31 (d, 3J60,50 = 5.6 Hz, 1H, H60), 8.99 (d, 3J6,5 = 5.6 Hz, 1H, H6), 8.92(s, 1H, H30), 8.52 (s, 1H, H3), 8.21 (d, 3J50,60 = 5.6 Hz, 1H, H50), 7.66(d, 3J5,6 = 5.5 Hz, 1H, H5), 2.67 (s, 3H, -CH3), 2.63 (s, 3H, -CH3(dmso)),2.61 (s, 3H, -CH3(dmso)). 1H NMR (d, 500 MHz, dmso-d6): 9.25 (d,3J60,50 = 5.5 Hz, 1H, H60), 9.04 (s, 1H, H30), 8.96 (d, 3J6,5 = 5.6 Hz, 1H,H6), 8.94 (s, 1H, H3), 8.14 (d, 3J50,60 = 5.7 Hz, 1H, H50), 7.69 (d,3J5,6 = 5.2 Hz, 1H, H5), 4.02 (s, 1H, -OH), 2.59 (s, 3H, -CH3). 13CNMR (d, 126 MHz, CD3NO2): 196.50 (s, COfac), 196.35 (s, COfac),191.30 (s, COfac), 164.35 (s, -COOH), 157.39 (s, C20), 154.89 (s,C40), 154.59 (s, C2), 154.25 (s, C60), 152.68 (s, C6), 142.04 (s, C4),128.94 (s, C5), 126.74 (s, C50), 125.19 (s, C3), 123.03 (s, C30), 37.64(d, 2C, -CH3(dmso)), 20.41 (s, -CH3). Selected IR bands (cm1, KBrpellets): 2029 (mCOfac), 1916 (mCOfac), 1710 (mCOacid), 947 (mSO),842 (mP-F), 558 (mP-F). UV-Vis (kmax, nm, CH2Cl2): 295, 318sh,331sh, 375., 103946-54-9
As the paragraph descriping shows that 103946-54-9 is playing an increasingly important role.
Reference£º
Article; Cavigli, Paolo; Balducci, Gabriele; Zangrando, Ennio; Demitri, Nicola; Amati, Agnese; Indelli, Maria Teresa; Iengo, Elisabetta; Inorganica Chimica Acta; vol. 439; (2016); p. 61 – 68;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI