15128-90-2
15128-90-2 結(jié)構(gòu)式
基本信息
5-HYDROXY-2-METHYL-6-NITROPYRIDINE
6-METHYL-2-NITRO-3-HYDROXYPYRIDINE
6-METHYL-2-NITRO-3-PYRIDINOL
3-Pyridinol, 6-methyl-2-nitro-
6-methyl-2-nitropyridin-3-ol
5-hydroxy-6-nitro-2-picoline
3-HYDROXY-6-METHYL-2-NITROPYRIDINE 99%
3-HYDROXY-2-NITRO-6-PICOLINE (3-HYDROXY-6-METHYL-2-NITROPYRIDINE)
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
Skin Irrit. 2
STOT SE 3
制備方法
1121-78-4
15128-90-2
以3-羥基-6-甲基吡啶為原料合成3-羥基-6-甲基-2-硝基吡啶的一般步驟:將3-羥基-6-甲基吡啶(23.6 g,216 mmol)溶于濃硫酸(50 mL)中,并冷卻至0℃。在1小時內(nèi)緩慢加入發(fā)煙硝酸(50 mL)。反應(yīng)混合物在室溫下攪拌1小時后,倒入冰(400 g)中,過濾收集沉淀。將所得固體溶解于乙酸乙酯中,用鹽水(100 mL)洗滌有機(jī)層。有機(jī)相經(jīng)無水硫酸鎂干燥后,減壓蒸發(fā)溶劑,得到標(biāo)題化合物12.1 g(產(chǎn)率36.3%)。產(chǎn)物熔點(diǎn)為102-105℃。1H NMR(DMSO-d6, 300 MHz)δ:2.44(s, 3H),7.52(d, J = 8.5 Hz, 1H),7.58(d, J = 8.5 Hz, 1H)。質(zhì)譜(ESI-Q1MS)m/e 153(M-H)+。元素分析計算值(C6H6N3O3):C, 46.76; H, 3.92; N, 18.18。實(shí)測值:C, 46.65; H, 3.98; N, 18.10。
參考文獻(xiàn):
[1] Heterocycles, 1994, vol. 38, # 3, p. 529 - 540
[2] Journal of Medicinal Chemistry, 1987, vol. 30, # 11, p. 2031 - 2046
[3] Patent: US6133253, 2000, A
[4] Patent: US5155116, 1992, A
[5] Patent: US5084456, 1992, A
