化学合成。
化学合成
合成路线 1(1. 合成:754230-78-9)
产率:81%
合成条件:With sulfuric acid; bromine; acetic acid In water at 0 - 4℃; for 4.50 h;
实验步骤:将2-氨基-3-苄氧基吡啶(85.0g,0.42mol)溶于10%硫酸水溶液(1000ml)中。将黄色溶液冷却至0至4℃并在2小时内滴加溴(80.5g,0.50mol)的乙酸(276g,4.6mol)溶液。得到红色悬浮液,将其在0℃下搅拌2.5小时,然后倒入冰水(500ml)和二氯甲烷(1000ml)的混合物中。通过向充分搅拌的两相混合物中加入25%氨水溶液(约600ml)来调节pH值为8。分离各相,水相用二氯甲烷(3×500ml)萃取。将合并的有机相用水(400ml)洗涤并用硫酸钠干燥。减压除去溶剂,残余物通过快速色谱法纯化[1kg硅胶,洗脱剂:石油醚/乙酸乙酯= 7:3(v / v)]。因此,分离出96.0g标题化合物,为棕色固体(81%收率)。熔点:109-110℃1H-NMR(CDCl3,200MHz):8 = 4.73(bs,2H),5.04(s,2H),7.08(d,1H),7.40(me,5) H),7.73(d,1H)。
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