化学合成。
化学合成; 医药
合成路线 1(1. 合成:94838-55-8)
产率:100%
合成条件:With palladium 10% on activated carbon; hydrogen In methanol at 20℃; for 2 h;
实验步骤:向28(590mg,2.33mmol)的甲醇(20.6mL)混合物中加入Pd / C(62mg; 10%pp)。 将反应混合物在35PSI压力下在室温下氢化2小时。 过滤反应混合物并蒸发。 通过硅胶柱色谱法(乙酸乙酯:正己烷= 1:1作为洗脱剂)纯化残余物,得到29(520mg; 100%),为油状物。 1H NMR(DMSO-d6):δ1.37(s,9H),3.91(d,J = 6.0Hz,2H),4.90(s,2H,用D2O处理消失),6.47(d,J = 8.1Hz, 2H),6.87(d,J = 8.0,2H),7.13ppm(s,1H,用D 2 O处理消失)。 IR:ν1695,2974cm-1。
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