With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.194800-56-1,[2,2′-Bipyridine]-4,4′-diyldiphosphonic acid,as a common compound, the synthetic route is as follows.
Dichloro-p-cymene ruthenium dimer (0.200 g, 0.320 mmol, 1.00 equiv.) was dissolved in degassed, dry DMF (122 mL). 4,4?-Bis(5-hexylthiophene-2-yl)-2,2?-bipyridin (0.310 g, 0.640 mmol, 2.00 equiv.) was added and the mixture was first stirred at 80 C for 4 h and then at room temperature for 12 h. Afterwards, dpbpy 7 (0.200 g, 0.640 mmol) was added and the reaction mixture stirred at 150 C for 4,5 h. After cooling to room temperature an excess of ammonium thiocyanate (2.02 g, 26.5 mol) was added, the mixture heated to 150 C and stirred for 4 h and then at room temperature for 12 h. The solvent was removed in vacuo, the crude product was precipitated with water, and subsequently purified by size exclusion chromatography on a Sephadex-LH 20 column. The desired complex was obtained as dark-red crystals (180.0 mg, 0.176 mmol, 27 %). 1H NMR (700 MHz, CD3OD): delta in ppm 8.96-8.92 (m, 2H), 8.83 (s, 1H), 8.13 (bs, 1H), 7.82 (d, J= 3.7, 1H), 7.74-7.73 (m, 1H), 7.70-7.62 (m, 4H), 7.54 (d, J= 6.3 Hz, 1H), 7.46 (dd, J= 6.0, 2.1 Hz, 1H), 7.37-7.335 (m, 1H). 7.17 (d, J= 5.8 Hz, 1H), 6.91 (d, J= 3.9, 1H), 2.86 (t, J= 7.6 Hz, 4H), 1.72 (p, J= 7.6 Hz, 4H), 1.42-1.31 (m, 12H), 0.90 (t, J= 7.0 Hz, 6H). 31P NMR (400 MHz; MeOD-d4): delta in ppm= 6.88 (s). HRMS (ESI) m/z: [M-2H]-2: calcd. for (C42H44N6O6S4P2Ru-2): 510.0367; found 510.0364. Anal. Calcd for RuC42H46N6O6P2S4: H, 4.54; C, 49.35; N, 8.22. Found: H, 5.01; C, 36.26; N, 5.64. IR (max, solid): 2921 nu(CH3), 2850 nu(H-O-P=O), 2096 nu(SCN), 1273 nu(NSC).
194800-56-1, The synthetic route of 194800-56-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Neuthe, Katja; Bittner, Florian; Stiemke, Frank; Ziem, Benjamin; Du, Juan; Zellner, Monika; Wark, Michael; Schubert, Thomas; Haag, Rainer; Dyes and Pigments; vol. 104; (2014); p. 24 – 33;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI