化学合成。
化学合成
合成路线 1(1. 合成:81196-09-0)
产率:94%
合成条件:Stage #1: With sodium carbonate In 1,4-dioxane; waterCooling with ice Stage #2: at 20℃; for 4 h;
实验步骤:通用方法:2-(4 - ((叔丁氧基羰基)氨基)苯基)乙酸(5)。 4-氨基苯乙酸(4,4g,26.46mmol,1当量)在二恶烷(52mL)和水(52mL)的混合物中的溶液,和碳酸钠(2.8g,26.42mmol,1当量, 在25mL水中搅拌并在冰浴中冷却。 一次性加入二碳酸二叔丁酯(BOC-酐,6.24g,28.59mmol,1.1当量),并在室温下继续搅拌4小时。 真空除去二恶烷,冷却水层,用乙酸乙酯层覆盖,用稀KHSO4酸化至pH4。 随后通过萃取(乙酸乙酯)并纯化(1:1:1)乙酸乙酯 - 己烷 - 乙酸; (乙酸乙酯),得到化合物5(方案7; 7.07g; 94%),为白色固体。 1H-NMR(300MHz,CDCl3):7.29(d,J = 8.40Hz,2H),7.19(d,J = 8.47Hz,2H),3.70(s,1H),3.58(s,2H),1.52( s,9H)。
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