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。
参考文献：
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合成路线 2（2. 合成：94838-55-8）
产率：95%
合成条件：With triethylamine In acetone at 20℃; for 16 h;
实验步骤：将7g（57.2mmol）4-氨基苄胺（市售），13.7g（63mmol）Boc 2 O和9.57ml（68.7mmol）NEt 3在100ml丙酮中的混合物用3.74g（17.1mmol）Boc 2 O进一步处理并在37℃下搅拌。 室温保持16小时。 蒸发所有挥发物后，残余物用乙酸乙酯萃取，有机部分用0.5N NaOH水溶液洗涤，用MgSO 4干燥。 蒸发溶剂，得到12.14（95％）标题化合物。 MS（m / e）：223.3（MH +，100％）
参考文献：
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