Related Products of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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.
In a 100 mE round-bottomed flask under argon, 1 g of 2-bromo-4-iodoroluene (3.37 mmol; 1 eq) and 0.51 g methyl azetidine-3-carboxylate, hydrochloride (preparation 1; 3.36 mmol; 1 eq) were dissolved in 10 mE of toluene. The solution was degassed with argon 4.39 g of cesium carbonate (13.47 mmol; 4 eq) 62mg of Pd2(dba)3 (0.07 mmol; 0.02 eq). and 117 g of Xant-Phos (0.20 mmol; 0.06 eq) were successively added and the reaction medium was stirred at 100 C. overnight. It was brought back to RT and diluted in EtOAc, then washed with watet The aqueous phase was extracted once again with EtOAc. The combined organic phases were dried over MgSO4, filtered and evaporated to give 1.15 g of a colorless oil. It was purified by flash chromatography on silica using a cyclohexane/0% to 10% EtOAc gradient, to give 510mg of the title compound in the form of a brown oil.Yld: 53%.?H NMR (300 MHz, DMSO-d5) oeppm 2.21 (s, 3H); 3.55-3.70 (m, 1H); 3.67 (s, 3H); 3.84-3.87 (m, 2H);3.97-4.03 (m, 2H); 6.39 (dd, J=8.4, 2.4 Hz, 1H); 6.65 (d, J=2.4 Hz, 1H); 7.13 (d, J=8.4 Hz, 1H).11015] LC-MS: m/z (M+H): 284.
The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; INVENTIVA; BOUBIA, Benaissa; MASSARDIER, Christine; GUILLIER, Fabrice; POUPARDIN, Olivia; TALLANDIER, Mireille; AMAUDRUT, Jerome; BONDOUX, Michel; FEENSTRA, Roelof Williem; VAN DONGEN, Maria Johana Petronella; (207 pag.)US2017/66717; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com