Electric Literature of 355-43-1, 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 355-43-1 as follows.
In a 25 mL round bottomed flask, was placed under N2 atmosphere a mixture of 2 (0.66 g, 2.0 mmol), perfluoro 1-iodohexane or perfluoro 1-iodooctane (2.5 mmol), AIBN (13 mg, 0.08 mmol) and 2 mL of 1,2-dichloroethane. The mixture was then stirred at 75C for 18 h. After cooling to room temperature, the solvent was removed under vacuum and the residue was subjected to a column chromatography on silica gel (ethyl acetate/hexane: 1/3) followed by a recrystallization in ethanol, to provide 3a and 3b as white solids. 4.3.1. 4′-{(4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluoro-2-iodononyl)oxy}-(1,1′-biphenyl)-4-yl benzoate (3a) Yield: 89%. 1H NMR (CDCl3) d 8.25 (d, 2H, J = 7.5 Hz), 7.5-7.7 (m,7H), 7.30 (d, 2H, J = 8.2 Hz), 7.0 (d, 2H, J = 8.5 Hz), 4.55 (quint., 1H, CHI), 4.21-4.38 (dd, 2H,2J = 10.5 Hz,3J = 4.8 Hz, CHICH2O), 2.85-3.23 (m, 2H, CF2CH2CHI). 13C NMR (CDCl3) d(ppm) 165.2(CO), 157.2 (ArO), 150.1 (ArO), 138.3, 134.2, 133.6, 130.2, 129.51, 128.5, 128.3, 127.8, 121.9, 115.2, 72.8 (CH2O), 37.8 (t,2JCF= 21 Hz, CF2CH2), 12.7 (CI). 19F NMR (CDCl3) d(ppm) 80.5 (t, CF3, 3JFF= 10.0 Hz), 113.1 & 113.3 (dm & dm, 21F, JA-B= 295 Hz, 2 diastereoisomers of CHICH2CF2), 121.5 (m, 2F), 122.6 (m,2F), 123.3 (m, 2F), 125.8 (m, 2F). HRMS (ESI) calculated for C28H18F13IO3Na+: 799.314 (found: 799.005).
According to the analysis of related databases, 355-43-1, the application of this compound in the production field has become more and more popular.
Reference:
Article; Marzouk, Samir; Khalfallah, Ali; Heinrich, Benoit; Khiari, Jamel Eddine; Kriaa, Abdelkader; Mery, Stephane; Journal of Fluorine Chemistry; vol. 197; (2017); p. 15 – 23;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com