- 3-氨基-6-吗啉基吡啶是一种吡啶类衍生物,可作为医药中间体,用于实验室有机合成过程中。
- 制备
步骤1:
室温下,将2-溴-5-硝基吡啶(2g,10mmol)加入到10毫升吗啉溶液中,室温下剧烈 搅拌4小时。反应结束后,有黄色固体析出。过滤后,以50毫升石油醚洗涤黄色固体,得到4- (5-硝基吡啶-2-基)吗啉(1.9g,92%)。波谱数据:MS m/z(ESI):210.1[M+H]+
步骤2:
室温下,将钯碳(100mg,10%wt)加入到4-(5-硝基吡啶-2-基)吗啉(1g,9.1mmol) 的60毫升甲醇溶液中,在氢气气氛下室温剧烈搅拌20小时。反应结束后,滤去钯碳,将滤液 减压浓缩,得到产物3-氨基-6-吗啉基吡啶,直接用于下一步反应。波谱数据:MS m/z(ESI): 180.1[M+H]+
医药中间体
合成路线 1(1. 合成:52023-68-4)
产率:100%
合成条件:With hydrogen In ethanol for 5 h;
实验步骤:含有1.65g(7.8mmol)4-(5-硝基-2-吡啶基)吗啉,160mg 5%Pt /碳和20ml的混合物。 将EtOH经50psi H 2 atm处理5小时。 将反应混合物通过硅藻土垫过滤,减压除去溶剂,得到1.4g(100%)6-(4-吗啉基)-3-吡啶胺,为紫色固体:1H NMR(400MHz,DMSO- c / 6)δ7.60(d,J = 2.9 Hz,1 H),6.92(dd,J = 8.8和2.9 Hz,1 H),6.62(d,J = 8.8 Hz,1 H),4.59(brs, 2 H),3.65-3.72(m,4 H)和3.17(dt,J = 4.9和2.4 Hz,4 H)。
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