91-16-7, name is 1,2-Dimethoxybenzene, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of 1,2-Dimethoxybenzene
Preparation A 1,2-dibromo-4,5-dimethoxybenzene 16.16 g of 1,2-dimethoxybenzene (117 mmol) are stirred at 0 C. in CCl4 (120 mL). 13.2 mL of dibromine (2.2 eq; 257.4 mmol; 41.13 g) dissolved in CCl4 (25 mL) are added dropwise (30 min) whilst monitoring the temperature (0-5 C.) [Fit an outlet which bubbles into a solution of Na2CO3 in order to neutralise the hydrobromic acid which forms]. After stirring for 2 hours at 0 C., the reaction mixture is then poured onto a mixture of water+ice, and the organic phase is washed with aqueous 10% NaHSO3 solution and then with aqueous 10% NaOH solution. After evaporation and drying, 33.42 g of a white solid corresponding to the title product are obtained. Yield=97% m.p. 92-93 C. 1H NMR (CDCl3): delta=7.06 (s; 2H); 3.86 (s; 6H). 13C NMR (CDCl3): delta=148.8; 115.9; 114.7; 56.2.
The synthetic route of 91-16-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Les Laboratoires Servier; Vaysse-Ludot, Lucile; Le Flohic, Alexandre; Vaultier, Michel; Pucheault, Mathieu; Kaminski, Thomas; US8859763; (2014); B1;,
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