Electric Literature of 1542-34-3,Some common heterocyclic compound, 1542-34-3, name is 3,5-Difluoro-4-iodoaniline, molecular formula is C6H4F2IN, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A suspension of 3,Sdifluoro4-4odoaniline (14.7 g, 55.9 mmol), CuT (0.745 g, 3.91 mmoi), bis(triphenyiphosphine)paiiadium(ll) dichioride (1 .59 g, 2,24 mrnoi), methyl 4 ethynylbenzoate (9.05 , 55.9 mmol), TEA (114 mL) and THF (44.1 mL) is stirred at 60Cfor 3 hr. The mixture is cooled to RT and the solvent evaporated to dryness under reduced pressure. EtOAc (10() mL) and H2() (100 mL) are added, and the resulting solid is filtered over diatornaceous earth. The organic layer from the filtrate is separated, dried over MgSO4, and evaporated to dryness under reduced pressure. A 1:1 mixture of DCM:heptane (400 nI) is added to the resulting residue and the mixture is stirred at RT overnight. The resultingsolid is collected by filtration and dried under vacuum to obtain the title compound (8.0 g,45.8% yield) as a brown solid. ?H NMR (300 MHz, DMSO-d6) oe 3.86 (s, 3H), 6.266.37 (m,4H), 7.59 (d, J = 8.2 Hz, 2H), 7.96 (d, J = 8.5 Hz, 2H).
The synthetic route of 1542-34-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ELI LILLY AND COMPANY; COATES, David Andrew; FALES, Kevin Robert; PETERSON, Jeffrey Alan; SCHKERYANTZ, Jeffrey Michael; SHEN, Quanrong; VALLI, Matthew John; WETTERAU II, John Rowley; WODKA, Dariusz Stanislaw; XU, Yangping; (118 pag.)WO2018/34883; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com