Synthetic Route of 5458-84-4, A common heterocyclic compound, 5458-84-4, name is 1-Iodo-2-methoxy-4-nitrobenzene, molecular formula is C7H6INO3, its 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.
Preparation XXXI-5-nitro-2-trifluoromethylanisole Cooled 140 mL pyridine in a large salable vessel to- [40 C.] Bubbled in trifluoromethyl iodide from a gas cylinder which had been kept in freezer overnight. After adding ICF3 for 20 min, added 2-iodo-5-nitroanisole (24.63 g) and copper powder (67.25 g). Sealed vessel and stirred vigorously for 22 h at [140 C.] After cooling [TO-50 C,] carefully unsealed reaction vessel and poured onto ice and [ET20.] Repeatedly washed with [ETZO] and H2O. Allowed the ice -Et2O mixture to warm to RT. Separated layers, washed organic layer with 1 N [HC1] (3x), then brine, dried over [NA2SO4,] filtered and concentrated in vacuo. Eluted material through silica gel plug (4.5 : 1 [HEX : CH2CL2)] to provide 5- nitro-2-trifluoromethylanisole.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; AMGEN INC.; WO2004/5279; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com