Downstream synthetic route of 194800-56-1

194800-56-1, The synthetic route of 194800-56-1 has been constantly updated, and we look forward to future research findings.

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