21901-41-7

基本信息
2-HYDROXY-5-NITRO-4-METHYL PYRIDINE
2-HYDROXY-5-NITRO-4-PICOLINE
4-METHYL-5-NITRO-2(1H)-PYRIDINONE
4-METHYL-5-NITRO-2-PYRIDINOL
4-METHYL-5-NITRO-2-PYRIDONE
5-NITRO-4-PICOLIN-2-OL
2-Hydroxy-4-Methyl-5-Nitropyri
2-HYDROXY-5-NITRO-4-PICOLINE (2-HYDROXY-4-METHYL-5-NITROPYRIDINE)
2(1H)-Pyridinone, 4-methyl-5-nitro-
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

21901-40-6

21901-41-7
以2-氨基-4-甲基-5-硝基吡啶為原料合成2-羥基-4-甲基-5-硝基吡啶的一般步驟:稱取2-氨基-4-甲基-5-硝基吡啶(10克,23毫摩爾)置于250毫升圓底燒瓶中,加入70毫升濃硫酸溶解,直至原料完全溶解。將反應(yīng)燒瓶置于-5℃的低溫冷浴中,通過恒壓滴液漏斗緩慢滴加預(yù)先配置的亞硝酸鈉(NaNO2,6.76克)水溶液。滴加過程中產(chǎn)生大量氣泡,需控制滴加速度以避免溫度迅速升高,確保反應(yīng)溫度不超過0℃。反應(yīng)過程中逐漸有固體析出。滴加完畢后,繼續(xù)攪拌10分鐘,反應(yīng)液變?yōu)槌壬⒊吻濉T?℃下繼續(xù)反應(yīng),通過薄層色譜(TLC)監(jiān)測(cè)反應(yīng)進(jìn)程。3小時(shí)后TLC顯示反應(yīng)完全,停止反應(yīng)。將反應(yīng)液緩慢倒入含有約300毫升水的燒杯中,析出大量黃色固體。室溫下靜置結(jié)晶3小時(shí)后,過濾收集固體,于紅外燈下干燥,得到6.72克黃色固體產(chǎn)物,收率為67.2%。
參考文獻(xiàn):
[1] Patent: CN105906621, 2016, A. Location in patent: Paragraph 0045
[2] Patent: EP2366691, 2011, A1. Location in patent: Page/Page column 13
[3] Journal of the Chemical Society, 1954, p. 2448,2455
[4] Journal of Organic Chemistry, 1955, vol. 20, p. 1729,1731
[5] Patent: WO2007/53394, 2007, A1. Location in patent: Page/Page column 12
報(bào)價(jià)日期 | 產(chǎn)品編號(hào) | 產(chǎn)品名稱 | CAS號(hào) | 包裝 | 價(jià)格 |
2025/05/22 | H1050 | 2-羥基-4-甲基-5-硝基吡啶 2-Hydroxy-4-methyl-5-nitropyridine | 21901-41-7 | 1G | 160元 |
2025/05/22 | H1050 | 2-羥基-4-甲基-5-硝基吡啶 2-Hydroxy-4-methyl-5-nitropyridine | 21901-41-7 | 5G | 730元 |
2024/08/19 | XW219014173 | 2-羥基-4-甲基-5-硝基吡啶 2-hydroxy-4-methyl-5-nitropyridine;2-hydroxy-5-nitro-4-picoline;4-methyl-5-nitro-2-pyridinol;5-nitro-4-picolin-2-ol;4-methyl-5-nitro-2(1h)-pyridinone;4-methyl-5-nitro-2-pyridone | 21901-41-7 | 25G | 176元 |