5221-37-4 2-氯-N-吡啶-2-基乙酰胺

危险等级:IRRITANT 海关编码:2933399990

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 +） 参考文献：

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合成路线 2（2. 合成：5221-37-4）

产率：80% 合成条件：With dicyclohexyl-carbodiimide In dichloromethane at 40℃; for 2 h; Inert atmosphere 实验步骤：将2-氨基吡啶（0.47g，5mmol）加入到氯乙酸（5mmol）的10mL CH 2 Cl 2溶液中。 在N 2下搅拌下，将所得混合物用DCC（1.03g，5mmol）的10mL CH 2 Cl 2溶液处理。 将该混合物在40℃保持2小时，然后在室温保持15分钟，过滤，用无水乙醚洗涤沉淀物。 蒸发浅棕色滤液，得到的黄棕色固体用SiO2色谱纯化，用二乙醚/乙酸乙酯洗脱，得到680mg（80％）白色晶体，暴露在空气中变成红紫色。 参考文献：

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