2-溴-4-叔丁基苯酚主要用于医药和农药领域,具体用途需结合具体应用场景进一步研究。
医药; 农药
合成路线 1(1. 合成:2198-66-5)
产率:100%
合成条件:With bromine In tetrachloromethane; chloroform at 0℃; Inert atmosphere
实验步骤:在2小时内将溴(7.18mL,0.14mol)的氯仿(25mL)溶液滴加到4-叔丁基 - 苯酚(20g,0.133mol)在1:1v / v氯仿中的溶液中: 在氮气下,在0℃下加入四氯化碳(64mL)直至持续出现轻微的红色着色(剩余约1mL溴溶液)。 然后将反应混合物用氮气吹扫过夜。 将得到的棕褐色溶液用二氯甲烷(50mL)稀释,用1%硫代硫酸钠水溶液(100mL)和饱和盐水(100mL)洗涤,干燥(MgSO 4),过滤并减压浓缩,得到2-溴-4 - (叔丁基)苯酚(30.5g,定量收率),为无色油状物。
参考文献:
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合成路线 2(2. 合成:2198-66-5)
产率:90%
合成条件:Stage #1: With toluene-4-sulfonic acid In methanol for 0.17 h; Stage #2: With N-Bromosuccinimide In methanol for 0.42 h;
实验步骤:一般步骤:将原料(~10mmol)和pTsOH(10mol%)在MeOH(1.0mL / mmol原料)中的溶液搅拌10分钟,然后搅拌NBS溶液(100mol%;从H 2 O重结晶) 在20分钟内从箔式反应烧瓶中滴加MeOH(0.1M)的MeOH溶液。 将反应混合物再搅拌5分钟,然后真空浓缩。 使用柱色谱(CH 2 Cl 2,或在CH 2 Cl 2中的1%MeOH)纯化得到的残余物。3.3。 产物表征2-溴-4-甲基苯酚(10)[23]:10.1mmol; 1.73克(92%);
参考文献:
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