作为医药中间体,用于抗生素、药物分子合成等医药相关研究。
医药
合成路线 1(1. 合成:87184-80-3)
产率:91%
合成条件:With sodium hypochlorite; 2,2,6,6-Tetramethyl-1-piperidinyloxy free radical; tetra(n-butyl)ammonium hydrogensulfate; potassium carbonate; potassium bromide In dichloromethane; water at 5 - 15℃; for 1 h;
实验步骤:5)5-(叔丁基 - 二甲基 - 硅烷氧基) - 戊醛的制备;向5-(叔丁基 - 二甲基 - 硅烷氧基) - 戊醇(16.8mmol,3.66g)的二氯甲烷(30mL)溶液中加入水(5.6mL),溴化钾(1.7mmol,202mg),n-在室温下,四丁基硫酸氢铵(0.84mmol,290mg)和TEMPO(30mg)。将得到的浅棕色溶液冷却至5℃并在该温度下滴加次氯酸钠(19.3mmol,30mL,5%)的溶液。加入一半次氯酸钠溶液后,加入固体碳酸钾(300mg)使反应混合物保持碱性。然后,在5-10℃下加入剩余的次氯酸钠溶液。此时,形成沉淀,并将反应混合物在10-15℃下再搅拌1小时。然后,加入水(100mL)。将得到的溶液萃取到乙醚(2.x.100mL)中。合并的有机萃取液用盐水溶液(150mL)洗涤,有机层用无水硫酸镁干燥。过滤干燥剂并除去溶剂,得到5-(叔丁基 - 二甲基 - 硅烷氧基) - 戊醛(3.32g,91%),为浅棕色油状物:ES(+) - HRMS m / e计算C11H24O2Si( M + H)+ 217.1619,发现217.1619。
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