3-溴-4-氨基苯甲酸乙酯主要作为医药中间体,用于相关药物分子的合成。
医药
合成路线 1(1. 合成:7149-03-3)
产率:91%
合成条件:With N-Bromosuccinimide In N,N-dimethyl-formamide at 0 - 20℃; for 18.50 h; Darkness
实验步骤:向在冰浴中冷却的DMF(150mL)的4-氨基苯甲酸乙酯(10g,61mmol)的溶液中分批加入NBS(10.8g,61mmol),并将混合物在相同温度下搅拌30分钟。 然后移去冰浴并在室温下继续搅拌过夜(18小时)。 将混合物倒入水(500mL)中并过滤,将橙色固体用水(50mL×2)洗涤并从EtOH中重结晶,得到浅黄色晶体(13.3g,91%)Rf = 0.38(PE:EtOAc = 5:1);熔点 86 - 88°C; 1H-NMR(CDCl3,300MHz)δ:8.07(s,1H),7.79(t,J = 11.55Hz,1H),6.70(d,J = 8.10Hz,1H),4.58(br,2H),4.37 (dd,J = 6.6Hz,J = 6.6Hz,2H),1.34(t,J = 7.2Hz,3H)。
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