89284-05-9

基本信息
4-氨基-3-硝基-5-溴吡啶
3-溴-4-氨基-5-硝基吡啶
4-氨基-3-溴-5-硝基吡啶
4-氨基-3-溴-5-硝基吡啶(CAS號:89284-05-9)
4-AMINO-3-BROMO-5-NITROPYRIDINE 4-氨基-3-硝基-5-溴吡啶
3-bromo-5-nitro-4-pyridinamine
4-AMino-3-nitro-5-broMopyridine
4-AMINO-3-BROMO-5-NITROPYRIDINE
3-Bromo-4-amino-5-nitropyridine
4-Pyridinamine, 3-bromo-5-nitro-
4-Amino-3-bromo-5-nitropyridine 97%
4-AMINO-3-BROMO-5-NITROPYRIDINE ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
制備方法

1681-37-4

89284-05-9
以4-氨基-3-硝基吡啶為原料合成4-氨基-3-溴-5-硝基吡啶的一般步驟如下:將3-硝基吡啶-4-胺(LXVIII)(10g,71.88mmol)與乙酸(100ml)混合于密封管中,隨后加入乙酸鈉(NaOAc)(29.50g,359mmol),并緩慢滴加溴(4.43ml,86.3mmol)。在攪拌條件下,將密封管于100℃加熱反應(yīng)過夜。反應(yīng)完成后,將混合物進行真空濃縮,所得固體溶于水,用飽和碳酸氫鈉(NaHCO3)水溶液堿化后,用二氯甲烷(DCM)進行萃取。合并有機相,經(jīng)干燥并濃縮,得到黃色固體3-溴-5-硝基吡啶-4-胺(LXIX)(13.7g,62.8mmol,收率87%)。產(chǎn)物經(jīng)1H NMR(DMSO-d6, 500MHz)鑒定:δ 8.58(s, 1H),9.19(s, 1H);ESIMS分析顯示分子離子峰m/z 218.1(M + H),對應(yīng)分子式C5H4BrN3O2。
參考文獻:
[1] Patent: US2013/296302, 2013, A1. Location in patent: Paragraph 0563
[2] Patent: WO2011/84486, 2011, A1. Location in patent: Page/Page column 119-120
[3] Patent: US2013/267495, 2013, A1. Location in patent: Paragraph 0460-0461
[4] Patent: EP2464232, 2015, B1. Location in patent: Paragraph 0087; 0088
[5] Patent: US2016/68548, 2016, A1. Location in patent: Paragraph 0852