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ChemicalBook CAS DataBase List 1,2,3,4-Tetramethylbenzene
488-23-3

1,2,3,4-Tetramethylbenzene synthesis

7synthesis methods
-

Yield:488-23-3 97.3%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran at 0 - 5;Inert atmosphere;Reflux;Temperature;Reagent/catalyst;

Steps:

1.5 Step 5: Synthesis process of 1,2,3,4-tetramethylbenzene
Under nitrogen protection, 3.8 g (0.1 mol) of lithium aluminum tetrahydride dissolved into 68 g of tetrahydrofuran and cooled at 0 to 5°C, after that added the drops of a mixture of 5.84 g (0.02 mol) of 1, 2-bis (bromomethyl)-3, 6-dimethylbenzene in 80 g of tetrahydrofuran, added the drops within 2 hours, and then it is warmed to reflux overnight, lowered at room temperature, and added 3.9 g of water and stirred for 45 minutes; again add 3.9g sodium hydroxide (15%) to separate the liquid, the organic phase is stirred for 30 minutes by adding 11.7 g of water and allowed to stand for stratification, the organic phase is dried over anhydrous magnesium sulfate, concentrate and obtained 2.61 g of product, yield 97.3%.

References:

Hangzhou Shengfutai New Materials Technology Co., Ltd.;Fu Chengfang CN107935804, 2018, A Location in patent:Paragraph 0021; 0025; 0030; 0040; 0045

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