These common heterocyclic compound, 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid, 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. category: iodides-buliding-blocks
Anhydrous dichloromethane (1.0 ml) and chloromethylenedimethyliminium chloride (76.8 mg, 0.600 mmol) were added to 2-iodo-5-methoxybenzoic acid (167 mg, 0.600 mmol) under ice cooling, and the resultant was agitated at room temperature for 30 minutes. A solution of 2-[(4-butylamino)benzo[d][1,3]dioxole]]-1,1,1,3,3,3-hexafluoropropan-2-ol (l) (72.0 mg, 0.200 mmol) dissolved in triethylamine (0.120 ml, 0.861 mmol) and dichloromethane (0.5 ml) was added to the reaction solution, and the mixture was agitated at room temperature for 20 hours. Water was added to the reaction solution, and an organic phase was extracted with ethyl acetate. The organic phase was washed with an aqueous solution of saturated sodium chloride, and the resultant was dried over sodium sulfate, followed by concentration under a reduced pressure. A crude product was purified via silica gel column chromatography using hexane:ethyl acetate (4:1) as an eluting solvent (yield: 123 mg, 99percent).
The synthetic route of 2-Iodo-5-methoxybenzoic acid has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Baba, Masanori; Hashimoto, Yuichi; Aoyama, Hiroshi; Sugita, Kazuyuki; Nakamura, Masahiko; Aoyama, Atsushi; Urata, Yasuo; US2012/316342; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com