用于医药、农药等领域的合成反应,无需进一步纯化即可用于下一步反应。
医药; 农药
合成路线 1(1. 合成:3883-58-7)
产率:93%
合成条件:Stage #1: With potassium hydroxide In 1,4-dioxane; waterHeating / reflux Stage #2: With hydrogenchloride In water at 120℃; for 0.25 h;
实验步骤:遵循公布的程序。 (Agosta,WC; Smith,ABJ Org.Chem.1970,35,3856)2-甲基-1,3-环戊二酮(10.025g,89.4mmol,Aldrich),甲基碘(6.0mL,96.4mmol,Aldrich)的混合物将KOH(5.097g,90.8mmol)的H 2 O(25mL)/二恶烷(75mL)溶液加热回流。 5小时后,加入KOH(2g)和MeI(2.4mL)的H 2 O(5mL)/二恶烷(15mL)溶液,再回流3小时后,将溶液在室温下搅拌过夜。早晨,通过加入KOH(2g)和MeI(2.4mL)的H 2 O(5mL)/二恶烷(15mL)溶液继续反应,并加热回流。 4小时后,将混合物冷却至室温,用乙醚(1×100mL,3→75mL)萃取。蒸发合并的乙醚萃取物,将残余物与HCl(50mL,10%)合并,并将所得混合物置于120℃油浴中直至观察到沸腾(约15分钟)。然后将混合物冷却至室温,通过加入NaHCO 3溶液(150mL,饱和)中和,然后用CH 2 Cl 2(4→75mL)萃取所得混合物。将合并的CH 2 Cl 2溶液干燥(MgSO 4),过滤并蒸发,得到棕色油状物(10.474g,83mmol,93%),将其直接用于下一步骤。
参考文献:
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