2-溴-1-环己基乙酮在医药领域有应用,具体用途未详细说明。
医药
合成路线 1(1. 合成:56077-28-2)
产率:100%
合成条件:With bromine In methanol for 2 h; Cooling with ice
实验步骤:步骤1.将2-溴-1-环己基乙酮将环己基甲基酮(0.30mL,2.4mmol)[Alfa Aesar cat L05501]溶于在冰浴和溴(0.38g,2.4mmol)中冷却的甲醇(3.0mL,74mmol)中。 )滴加了。 将混合物搅拌2小时,然后加入水(3.0mL)并将反应混合物搅拌4小时。 用EtOAc:己烷(3:1)萃取反应混合物。 合并的有机层用水饱和碳酸钾,盐水洗涤,用硫酸镁干燥并浓缩,得到2-溴-1-环己基乙酮,为透明油状物(0.49g,100%)。 NMR(300MHz,CDCl 3)δ3.96(s,2H),2.86-2.55(m,1H),2.24-1.08(m,10H)。
参考文献:
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合成路线 2(2. 合成:56077-28-2)
产率:85%
合成条件:With water In 1,2-dichloro-ethane at 20℃; for 14 h;
实验步骤:通用方法:向卤代炔(0.5mmol)的DCE(5mL)溶液中加入H 2 O(27mg,1.5mmol)和MCM-41-PPh 3-AuNTf 2(58mg,0.015mmol)。 将反应混合物在室温下搅拌,并使用TLC监测反应进程。反应通常需要14小时。 反应完成后,通过简单过滤反应溶液分离催化剂,用丙酮(25mL)洗涤,并在下一次运行中重新使用。 减压浓缩滤液,并使用硅胶色谱法(洗脱液:轻质石油醚/乙酸乙酯= 25:1)纯化残余物,得到所需产物2a-2b'。
参考文献:
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合成路线 3(3. 合成:56077-28-2)
产率:78%
合成条件:With hydrogen bromide In hexane; water at 20℃; for 2 h;
实验步骤:将得到的环己基重氮甲基酮溶解在己烷(8.2mL)中,缓慢加入HBr(0.69mL的48%HBr水溶液,6.16mmol HBr,1.5当量),观察到剧烈的鼓泡。 将溶液在室温下搅拌2小时后,加入饱和NaHCO 3溶液(5mL)并将混合物再搅拌5分钟,用H 2 O(3×10mL)洗涤,并经无水Na 2 SO 4干燥。 过滤并浓缩,得到纯的2-溴-1-环己基乙酮20(660mg,3.23mmol,78%),为浅黄色液体。
参考文献:
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