2-氯-N-吡啶-2-基乙酰胺主要作为医药中间体,用于相关药物的合成研究,在多个医药相关研究文献和专利中被提及,具有较高的合成价值和应用潜力。
医药
合成路线 1(1. 合成:5221-37-4)
产率:97%
合成条件:Stage #1: at 80℃; for 0.08 h; Microwave irradiation Stage #2: With sodium hydroxide In water; 1,2-dichloro-ethane
实验步骤:将2-氨基吡啶(2.8g,30mmol)溶于50ml玻璃容器中的二氯乙烷(25ml)中,并向其中滴加氯乙酰氯。 将玻璃容器用TFM特氟隆盖盖住并置于微波反应器中的转子中。 将混合物在300W和80℃下通过微波照射5分钟。 照射5分钟后,用饱和的氢氧化钠水溶液将反应混合物调节至pH9,并用二氯乙烷萃取两次。 将有机层用无水硫酸钠干燥。 用旋转蒸发器除去溶剂,用乙腈重结晶得到4.9g(97%)所需的粉红色固体产物。 熔点110-115℃。 IR(KBr)3443,3226,1683,1581,1330,1198,775cm -1; 1H NMR(CDCl3)4.2(2H,s),7.1(1H,d),7.7(1H,t),8.2(1H,d,J = 8.3Hz),8.4(1H,d,J = 4.9Hz), 8.95(1H,bs); 13C NMR(CDCl3)43.2,111.4,121.0,139.1,148.2,150.7,164.9; EIMS m / z 170.6(M +)
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