Reference of 2468-56-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2468-56-6 as follows.
Scheme 6. Preparation of HV As depicted in Scheme 6, a mixture of 4,4′-bipyridine (1.0 g, 6.4 mmol) and 6-iodo-l- hexyne (4.6 g, 22 mmol) in dry MeCN (30 mL) was heated at 105 C / 6 psi under N2 for 3 h. The reaction mixture was cooled to room temperature and the resulting reddish precipitate was filtered and washed thoroughly with MeCN. The solid was dissolved in H2O (100 mL), followed by the addition of excess of NH4PF6, resulting in the precipitation of an off-white solid which was collected by centrifugation, washed with H2O (3 x 20 mL), MeOH (1 x 20 mL) and dried in vacuo to yield HV 2PFe as a light brown solid (2.4 g) in 62% yield. NMR (500 MHz, CD3CN, 298 K) d = 8.90 (d, J= 6.4 Hz, 4H), 8.39 (d, J= 6.4 Hz, 4H), 4.65 (t, J= 7.5 Hz, 4H), 2.28 (dt, J= 2.6 Hz, J = 7.0 Hz, 4H), 2.23 (t, j = 2.6 Hz, 2H), 2.13 (p, j = 7.6 Hz, 4H), 1.60 (p, J = 7.4 Hz, 4H). 13C NMR (125 MHz, CD3CN, 298 K) d = 150.9, 146.5, 128.2, 84.2, 70.5, 62.5, 31.0, 25.5, 18.2. ESI-HRMS calcd for [M- PF6]+m/z = 463.1732, found 463.1740.
According to the analysis of related databases, 2468-56-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; NORTHWESTERN UNIVERSITY; KING ABDULAZIZ CITY FOR SCIENCE AND TECHNOLOGY (KACST); NGUYEN, Minh, T.; STODDART, James, Fraser; (82 pag.)WO2019/195754; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com