20469-65-2, 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 20469-65-2 as follows.
1-iodo-3,5-dimethoxybenzene:A dried round bottom flaks was charged with 1-bromo-3,5-dimethoxy- benzene (15.0 g, 69.1 mmol) and dry tetrahydrofuran (275 cm3). The resulting solution was cooled down to -78 0C, then n-butyllithium (2.5 M in hexanes, 29.0 cm3, 72.6 mmol) was added dropwise over 10 minutes. The mixture was stirred at -78 0C for 1 hour, then 1,2-iodoethane (20.5 g, 72.6 mmol) in dry tetrahydrofuran (75 cm3) was added rapidly to the solution. After an additional 1 hour at -78 0C, the resulting mixture was warmed to room temperature and stirred overnight. The mixture was poured into saturated sodium thiosulfate solution (200 cm3), extracted with diethyl ether four times and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the residue was recrystallized from methanol to obtain the title product as a white crystalline solid(13.0 g, yield 71 %). NMR (1H, 300 MHz1 CDCI3) : delta 6.85 (d, J = 2.3 Hz, 2H); 6.40 (t, J = 2.3 Hz, 1 H); 3.76 (s, 6H).
According to the analysis of related databases, 1-Bromo-3,5-dimethoxybenzene, the application of this compound in the production field has become more and more popular.
Reference:
Patent; MERCK PATENT GMBH; BLOUIN, Nicolas; MITCHELL, William; WANG, Changsheng; TIERNEY, Steven; WO2011/18144; (2011); A2;,
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