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以2,3,5,6-四氯对苯二甲腈为原料,经氟化、水解、酰化、还原、甲醚化五步反应,合成2,3,5,6-四氟-4-甲氧基甲基苯甲醇,反应总收率55%,产物纯度99%以上。着重对中间体2,3,5,6-四氟对苯二甲醇经选择性甲醚化合成2,3,5,6-四氟-4-甲氧基甲基苯甲醇的反应进行研究,得到优化的工艺条件:以硫酸二甲酯作为甲基化试剂,氢氧化钠为反应碱、甲苯为有机溶剂,硫酸二甲酯的物质的量为原料2,3,5,6-四氟对苯二甲醇的1.3倍,反应温度40~50℃。合成工艺具有反应步骤短,反应总收率高,污染排放少等优点,适合工业化生产。
With 2,3,5,6-tetrachloroterephthalonitrile as raw material, the fluorinated, hydrolyzed, acylated, reduced, methyl etherified five-step reaction to synthesize 2,3,5,6-tetrafluoro-4 - methoxymethyl benzyl alcohol, the total yield of 55%, product purity of more than 99%. The reaction of 2,3,5,6-tetrafluoroterephthalic acid with 2,3,5,6-tetrafluoro-4-methoxymethylbenzyl alcohol by selective methyl etherification was studied emphatically. Get the optimized process conditions: dimethyl sulfate as a methylating agent, sodium hydroxide as a reaction base, toluene as an organic solvent, the amount of dimethyl sulfate material as a raw material 2,3,5,6-tetrafluoride 1.3 times the amount of xylene, the reaction temperature is 40 ~ 50 ℃. The synthesis process has the advantages of short reaction steps, high total reaction yield, less pollution emission and the like, and is suitable for industrialized production.