Related Products of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.
2,4,6-trimethyliodobenzene (12 mmol, 3 equiv), elemental selenium (12 mmol, 3 equiv), 5-methylbenzoxazole (4 mmol, 1 equiv), Cu(OAc) 2 (at room temperature) 0.4 mmol), ammonium hydrogencarbonate (12 mmol, 3 equiv) was added to the reaction tube, then filled with nitrogen, and replaced three times. Under a nitrogen reaction environment, 20 mL of DMF reaction solvent was then added, and the mixture was stirred at a reaction temperature of 140 ° C for 24 hours. After monitoring the reaction by thin layer chromatography, the reaction mixture was cooled, then diluted with ethyl acetate, and the diluted solution was transferred to a separating funnel, and extracted with saturated brine to separate the aqueous and organic phases, and then acetic acid. The aqueous phase was extracted three times with ethyl acetate. The organic phase was combined, 25 g of anhydrous sodium sulfate was added, and the mixture was allowed to stand for 30 min, and the filter cake was washed three times with 50 mL of ethyl acetate each time, then the solvent was spun off, and the product was separated by column chromatography. Deprotection: petroleum ether: diethyl ether = 98:2), yield 90percent, product weight 1.191 g.
The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Wenzhou Medical University; Wu Ge; (9 pag.)CN108484518; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com