With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.56100-22-2,6-Methyl-2,2′-bipyridine,as a common compound, the synthetic route is as follows.
A colourless solution of 6-Mebpy (43 mg, 0.25 mmol) and BIPHEP (131 mg, 0.25 mmol) in CH2Cl2(20 mL) was added to a colourless solution of [Cu(MeCN)4][PF6] (93 mg, 0.25 mmol) in CH2Cl2 (20 mL),turning the solution yellow. After stirring at room temperature for 2 h, the solvent was removed underreduced pressure. The crude product was redissolved in CH2Cl2 and layered with Et2O, to precipitate[Cu(BIPHEP)(6-Mebpy)][PF6] (202 mg, 0.23 mmol, 92%) as a yellow powder. 1H-NMR (500 MHz,acetone-d6, 298 K): /ppm 8.72 (dt, J = 8.3, 1.0 Hz, 1H, HA3), 8.62 (d, J = 7.9 Hz, 1H, HB3), 8.29-8.21(overlapping m, 2H, HB4+A4), 8.04 (dt, J = 5.2, 0.8 Hz, 1H, HA6), 7.73 (dd, J = 7.8, 0.9 Hz, 1H, HB5),7.54 (m, 1H, HA5), 7.46-7.10 (overlapping m, 26H, HD2+D2?+D3+D3?+D4+D4?+C4+C4?+C5+C5?+C6+C6?), 6.99(m, 1H, HC3/C3?), 6.88 (m, 1H, HC3/C3?), 2.58 (s, 3H, HMe). 13C{1H} NMR (126 MHz, acetone-d6, 298 K):/ppm 160.5 (CB6), 153.5 (CA2/B2), 152.7 (CA2/B2), 151.0 (CA6), 145.7 (br, CC1+C1?), 140.6 (CA4/B4), 140.2(CA4/B4), 136.2 (br, CC6/C6?), 135.2 (br, overlapping, CD2/D2?), 134.2 (CD2/D2?), 134.1 (CD2/D2?), 129.45(CD3/D3?), 129.4 (CD3/D3?), 128.8 (br, CC4+C4?), 127.6 (CB5), 127.0 (CA5), 123.9 (CA3), 121.4 (CB3); signalsfor CC3, CC5, CC1, CC2, CD1 were poorly resolved. 31P{1H} NMR (202 MHz, acetone-d6, 298 K): /ppm1.3 (broad, FWHM = 428 Hz, BIPHEP) 3.7 (broad, FWHM = 401 Hz, BIPHEP), 144.2 (septet,JPF = 700 Hz, [PF6]). ESI MS: m/z 755.16 [M-PF6]+ (base peak, calc. 755.18). Found C 61.89, H 4.83,N 3.38; C47H38CuF6N2P3H2O requires C 61.41, H 4.39, N 3.05.
56100-22-2 6-Methyl-2,2′-bipyridine 639521, acatalyst-ligand compound, is more and more widely used in various.
Reference£º
Article; Keller, Sarah; Bantle, Matthias; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; Molecules; vol. 24; 21; (2019);,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI