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作 者:石强[1] 张翠娥[1] 刘敏[1] 邱少君[1] 余李敏[2] 刘洁[2] 肖志强[2]
机构地区:[1]西安近代化学研究所,陕西西安710065 [2]陕西新药技术开发中心,陕西西安710075
出 处:《应用化工》2011年第4期645-647,651,共4页Applied Chemical Industry
摘 要:采用分步法制备了2-甲基间苯二酚,反应分4步进行,间苯二酚与叔丁醇在浓硫酸存在下反应,得到4,6-二叔丁基间苯二酚(4);(4)、甲醛、二甲胺发生Mannich反应,制得2-二甲氨基甲基-4,6-二叔丁基间苯二酚(3);(3)在Pd/C催化下氢解,得到2-甲基-4,6-二叔丁基间苯二酚(2);(2)在AlCl3作用下,脱去叔丁基,得到目的产物2-甲基间苯二酚(1)。对各步骤反应条件进行了优化,(1)的总收率62.3%,纯度99.8%。对反应中间体及目的产物进行了IR或1HNMR表征。2-Methylresorcinol was synthesized by a four-step reaction.First,4,6-di-t-butylresorcinol(4) was synthesized from resorcinol and tert-butanol in the presence of concentrated sulfuric acid.Then,2-[(dimethylamino)methyl]-4,6-di-t-butylresorcinol(3) was synthesized from(4),formaldehyde and dimethylamine by Mannich reaction.2-Methyl-4,6-di-t-butylresorcinol(2) was synthesized from(3) by hydrogenolysis using Pd/C as the catalyst.Finally,2-methylresorcinol(1) was obtained by debutylization reaction of(2),using AlCl3 as a catalyst.The process was optimized,and(1) was synthesized in total yield of 62.3% and purity of 99.8%.The intermediates and the desired product were characterized by IR or 1H NMR respectively.
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