生命科学。
医药生物化工
合成路线 1(1. 合成:4270-27-3)
产率:97%
合成条件:Stage #1: With sodium hydroxide In water for 1 h; Reflux Stage #2: With hydrogenchloride In water
实验步骤:将含有NaOH(8.9g,0.22mol)的2,4,6-三氯嘧啶(11)(10.21g,0.56mol)在水(100mL)中的溶液在回流下搅拌1小时。 用浓盐酸将反应混合物调节至pH 2-3。 用HCl水溶液保存在冰箱中过夜。 过滤收集沉淀物,用冷水洗涤并在五氧化二磷上真空干燥。 得到6.43g(0.54mol,97%)6-氯尿嘧啶(6 {1,1}),为白色结晶固体。 光谱数据与文献报道的相同[28]和[40]。熔点 > 280°C。 1H NMR(300MHz,DMSO-d6)δ(ppm):12.00(br s,1H,NH),11.09(br s,1H,NH),5.66(s,1H,CH)。 IR(KBr,νcm-1):3095(N-H),1729,1709,1652(CO),1616(CC),1380(C-N),841(N-H),790(C-Cl)。
参考文献:
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