3-甲基-4-硝基吡啶 N-氧化物是重要的精细化工中间体,在医药工业上主要用于制备轻吡头孢菌素(Compound6f)等。
医药
合成路线 1(1. 合成:1074-98-2)
产率:50%
合成条件:at 0 - 100℃; for 2 h;
实验步骤:步骤b:合成3-甲基-4-硝基吡啶1-氧化物-3-甲基吡啶1-氧化物(2g,18.3mmol,步骤a)缓慢加入到含有硫酸(7mL,128mmol)的圆底烧瓶中。 将混合物冷却至0℃并逐滴加入硝酸(5.7mL,128mmol)。 将所得反应混合物在90-100℃下加热2小时。 将反应混合物倒入碎冰中,分批加入碳酸钠。 用氯仿萃取水相。 将合并的有机层用盐水洗涤,用无水硫酸钠干燥并在真空下浓缩,得到3-甲基-4-硝基吡啶1-氧化物(1.4g,50%)。1 H NMR(400MHz,CHCl 3 -cc): δ8.09-8.17(m,2H),8.02(d,J = 7.09Hz,1H),2.62(s,3H)。
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