Reference of 32024-15-0,Some common heterocyclic compound, 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, molecular formula is C9H9IO3, 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.
General procedure: Selected base (1.5×10-4 mol, 1.5 equivs), aryl iodide (1.0×10-4 mol, 1.0 equiv) and terminal alkyne (1.0×10-4 mol, 1.0 equivs) were mixed in a 10-mL vial, followed by addition of a solution of the selected catalyst (1×10-8 mol) in EtOH (1 mL). The vial was placed in a pre heated oil bath at 80 C and stirred for 4 h. After cooling to ca. 25 C, the reaction mixture was evaporated to dryness under a stream of dinitrogen followed by addition of 1.0 equivof 1,2-dimethoxyethane (NMR internal standard), and extraction of the reaction mixture with three 0.20 mL portions of CDCl3. All fractions were joined and analyzed by 1H NMR spectroscopy. The product peak assignments were based on authentic samplesor on published data [56,62-68] (several sources were used for published compounds), while the structure of two new products,i.e. 3,4-dimethoxy-5-(phenylethynyl)benzaldehyde (derived from the coupling of 3-iodo-4,5-dimethoxybenzaldehyde with phenylacetylene) and 1-fluoro-2-[(2-methylphenyl)ethynyl]benzene (prepared from 2-fluorophenylacetylene and 2-iodotoluene were undoubtedly established using NMR spectroscopy, MS and elemental analyses (see Supplementary data). Quantifications were performed upon integration of the selected peak of the product in the 1H NMR relatively to the peak of the standard.
The synthetic route of 32024-15-0 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Valishina, Elena A.; Silva, M.Fatima C. Guedes Da; Kinzhalov, Mikhail A.; Timofeeva, Svetlana A.; Buslaeva, Tatyana M.; Haukka, Matti; Pombeiro, Armando J.L.; Boyarskiy, Vadim P.; Kukushkin, Vadim Yu.; Luzyanin, Konstantin V.; Journal of Molecular Catalysis A: Chemical; vol. 395; (2014); p. 162 – 171;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com