合成路线 1(1. 合成:657-15-8)
产率:89%
合成条件:at 0℃; for 1 h;
实验步骤:将2,2,2-三氟苯乙酮(0.5mL,3.68mmol)溶解在硫酸(3mL)中,并加入NaNO 3(0.31g,3.68mmol)。 将反应溶液在0℃下搅拌约1小时。 通过加入5N NaOH水溶液校准反应混合物,使pH值为8-9。 将反应混合物用氯仿/ 2-丙醇= 4/1(v / v)稀释,并用蒸馏水洗涤。 将有机层用无水硫酸钠干燥,过滤,并减压浓缩。 使用硅胶色谱法纯化浓缩的化合物,得到标题化合物(720mg,89%)。 -NMR光谱(300MHz,DMSO-MS(ESI +,m / z):220 [M + H] +
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