化学合成。
化学合成
合成路线 1(1. 合成:61032-41-5)
产率:99%
合成条件:at 0℃; for 1.67 h;
实验步骤:将甲基-4-苄氧基-3-甲氧基苯甲酸酯(5.00g,18.4mmol)溶解在Ac 2 O(23.5mL)中并冷却至0℃。 过量分批加入Cu(NO 3)2(5.05g,27.0mmol)。 在90分钟后,LCMS表明产物形成。 将混合物倒入冰水中并搅拌45分钟。 通过离心回收粗产物,用水冲洗并干燥。 使用石油醚/乙酸乙酯梯度,通过在Combiflash系统上的硅胶色谱法纯化粗产物。 5.80克(99%),灰白色固体。 1 H NMR(CD3OD,ö以ppm计):7.62(s,1H),7.45(d,2H),7.40(t,2H),7.35(m,1H),7.25(s,1H),5.20(s, 2H),3.95(s,3H),3.90(s,3H)。 MS(ESI-QMS):m / z = 318.03(M + H)。
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