5471-81-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 5471-81-8 as follows.
Under a protective atmosphere of inert gas, Pd(OAc)2 (2.2 mg, 10 mol%), XPhos (19.1 mg, 20 mol%), NBE-CO2K (3.5 mg, were added to a 4.0 mL reaction flask equipped with a magnetic stir bar. 10 mol%), 3-methyl-4 iodine benzoate Methyl ester (0.2 mmol, 1.0 equiv.), 1,2-epoxyoctadecane (0.6 mmol, 3.0 equiv.) and dry N-methylpyrrolidone (1.0 mL). The reaction flask was capped and stirred at room temperature for about 5 minutes, after which the mixture was heated to 80 C and stirred 24hour. After the reaction vessel was cooled to room temperature, it was quenched with water (10 mL), extracted with methyl tert-butyl ether (3¡Á10 mL), dried Na2SO4 Dry, filter, and concentrate under vacuum. Purified by column chromatography, the eluent was petroleum ether: ethyl acetate = 50:1 (v/v),67 mg of methyl 7-methyl-2-n-hexadecyl-2,3-dihydrobenzofuran-5-carboxylate (white solid, yield 80%).
According to the analysis of related databases, Methyl 4-iodo-3-methylbenzoate, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Wuhan University; Zhou Qianghui; Wu Chenggui; Cheng Honggang; (20 pag.)CN108329285; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com