化学合成。
化学合成
合成路线 1(1. 合成:135034-10-5)
产率:100%
合成条件:With hydrogen iodide; sodium iodide In hexane at 40℃; for 4 h; Inert atmosphere
实验步骤:例35; 3-氯-6-碘 - 哒嗪(103); 将3,6-二氯哒嗪(46)(2g,13.42mmol),碘化钠(2g,13.42mmol)和氢碘酸(10mL)在氩气氛中在40℃下加热4小时的混合物。 回到室温后,将反应介质倒在冰上,加入浓缩的钠溶液,搅拌混合物10分钟。 然后用DCM萃取溶液。 将有机相用水洗涤,用Na 2 SO 4干燥,过滤并在真空下浓缩。 得到La 3-氯-6-碘 - 哒嗪(103),为黄色粉末(3.20g,定量)。1H H RMN(CDCl3)δ(ppm):7.35(d,J = 9.0,2H,Hpyridazine) ),8.38(d,J = 9.0,2H,Hpyridazine).13C RMN(CDCl3)δ(ppm):122.9,129.2,139.2,157.1.MS,m / z(1%):240(M +,18%), 127(I +,100%)。
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