101990-45-8 2-溴-5-(溴甲基)吡啶

危险品运输编号:UN 3335 WGK Germany:3 海关编码:2933399990

未明确提及具体用途，主要作为中间体用于相关领域合成。

医药; 农药

合成路线 1（1. 合成：101990-45-8）

产率：89% 合成条件：With N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile) In 1,2-dichloro-ethane at 85℃; for 0.50 h; 实验步骤：（参考例8）2-溴-5-（溴甲基）吡啶（参考化合物8）的合成N-溴代琥珀酰亚胺（16g，91mmol）和0.40g（2.4mmol）2,2'-偶氮二（异丁腈）的合成加入到12g（70mmol）2-溴-5-甲基吡啶在100ml 1,2-二氯乙烷中的溶液中，并将混合物在85℃下搅拌。 15分钟后，向其中加入0.40g（2.4mmol）2,2'-偶氮双（异丁腈）并将混合物搅拌15分钟。反应结束后，在反应溶液中加入水，分离有机层。将有机层用无水硫酸镁干燥并真空浓缩。将所得残余物进行硅胶柱色谱（不含溶剂：正己烷：乙酸乙酯= 10：1至9：1（v / v）），将含有目标物质的部分真空浓缩，得到15g标题化合物，为白色粉末（收率：89％）。 Rf值：0.63（正己烷：乙酸乙酯= 9：1（v / v））质谱（CI，m / z）：250,252,254（M + +1）1H-NMR谱（CDCl3，δppm） ）：4.42（s，2H），7.49（d，J = 8.3Hz，1H），7.61（dd，J1 = 8.3Hz，J2 = 2.7Hz，1H），8.39（d，J = 2.7Hz，1H） 参考文献：

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