With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.168646-54-6,5,6-Diamino-1,10-phenanthroline,as a common compound, the synthetic route is as follows.
[Cu(CH3CN)4]ClO4 (32.6 mg, 0.100 mmol) was added to a DCMsolution (about 12 mL) of dap (10.7 mg, 98percent, 0.0500 mmol) andxantphos (59.0 mg, 98percent, 0.100 mmol) under a stream of dry argonby using Schlenk techniques at room temperature and a vacuumlinesystem, then orange-red solution was obtained quickly andstirred for 1 h at room temperature. The above process can alsobe carried out in air with the existence of oxygen. After filtrationthrough absorbent cotton, layering n-hexane onto the DCM solutionin air produced the product as bluish violet to black-blue blockcrystals in 76percent yield (63.0 mg). Anal. Calc. for C90H72Cl2Cu2N4O10P4(1b): C, 63.97; H, 4.30; N, 3.32. Found: C, 64.25; H, 4.35; N, 3.26percent.ESI-MS (m/z): 1589.25 {[Cu2(l-pdi)(xantphos)2]ClO4}+ (calcd1589.27); 849.1963 [Cu(pdi)(xantphos)]+ (calcd 849.1968);745.153 [Cu2(l-pdi)(xantphos)2]2+ (calcd 745.159); 641.1222[Cu(xantphos)]+ (calcd 641.1224). 1H NMR (400 MHz, DMSO-d6,delta, ppm): 13.190 (s, 2H, CNH), 9.030 (d, 2H, J = 8.0 Hz), 8.452 (d,2H, J = 4.8 Hz), 7.888 (dd, 2H, J = 8.0 Hz, J0 = 1.2 and 0.8 Hz),7.846?7.814 (m, 4H), 7.340?7.149 (m, 36H), 6.983?6.938 (m, 8H),6.729?6.694 (m, 2H), 6.650?6.615 (m, 2H), 1.732 (s, 6H, CH3),1.653 (s, 6H, CH3). 31P{1H} NMR (400 MHz, DMSO-d6, delta, ppm):5.980, 12.816. Characteristic IR spectrum (KBr, cm-1): 3258m(NH), 2961m (CH3), 2923w (CH3), 2858w (CH3); 1097s (ClO4).
168646-54-6, The synthetic route of 168646-54-6 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Yao, Xi-Xi; Guo, Ya-Meng; Liu, Rong; Feng, Xiao-Yan; Li, Hao-Huai; Liu, Nian; Yang, Feng-Lei; Li, Xiu-Ling; Polyhedron; vol. 92; (2015); p. 84 – 92;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI