494-99-5, name is 1,2-Dimethoxy-4-methylbenzene, 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. Product Details of 494-99-5
3,4-Dimethoxytoluene (7.6 g, 50 mmol),Sodium bromate (6.0g, 40mmol),Sodium Bromide (8.2g, 80mmol)And carbon tetrachloride (18mL),Add to stirReturn condenser,In the reaction flask of thermometer and tail gas absorption device,Heat to reflux,Slowly add 1/2 volume of sulfuric acid (60mmol of concentrated sulfuric acid is diluted with 2mL of water and added within about 1.5h).Followed by gas chromatography,After the substrate is fully involved in the reaction (about 1 h),Quickly add 1/3 volume of initiator solution (1.12g ABVN dissolved in 7mL carbon tetrachloride),After the emergence of a vigorous reflux system,Continue to slowly add the remaining sulfuric acid and initiator solution (approx. 4.5 hours later),Continue the reaction until the product is no longer formed or the byproduct is significantly increased (about 1.5 h),To room temperature,filter,The filtrate was washed with 10 ml of sodium bicarbonate solution (5%).Liquid separation,The organic phase is dried over anhydrous sodium sulfate.concentrate,The crude product was purified by recrystallization (ethyl acetate:petroleum ether=1:13, volume ratio) to give 2-bromo-4,5-dimethoxybenzyl bromide (13.08 g).Yield 85%.
The synthetic route of 494-99-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Zhejiang Normal University; Xiao Xiaohui; Chen Yufeng; (9 pag.)CN107417501; (2017); A;,
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