26456-59-7

基本信息
5-羥基嘧啶
5-羥基嘧啶 1KG
5-羥基嘧啶 (醋酸鹽)
pyrimidin-5-ol
5-Hydroxypyrimidine
5-Hydroxypyrimidine ,98%
5-Hydroxypyrimidine acetate
5-HydroxypyriMidine. AcOH salt
5-Pyrimidinol (6CI,7CI,8CI,9CI)
Pyrimidin-5-ol, 5-Hydroxy-1,3-diazine
物理化學(xué)性質(zhì)
制備方法

31458-33-0

26456-59-7
以5-甲氧基嘧啶為原料合成5-羥基嘧啶的一般步驟:將5-甲氧基嘧啶(2.99g,27.2mmol)與粉末狀氫氧化鉀(8.96g,85%,136mmol)在甲醇(50mL)中的混合物置于密封管中,于150℃下加熱反應(yīng)過夜。反應(yīng)完成后,將混合物冷卻至室溫,加入乙酸進(jìn)行中和,隨后在減壓條件下濃縮。所得殘余物用熱乙腈(2×100mL)研磨,合并乙腈萃取液并減壓濃縮,得到7.51g灰白色固體。將該固體用熱乙酸乙酯(100mL)研磨,減壓濃縮乙酸乙酯萃取液,得到1.81g灰白色固體。最后,通過快速色譜法(硅膠為固定相,9:1的二氯甲烷/甲醇為流動(dòng)相)進(jìn)一步純化,得到目標(biāo)產(chǎn)物5-羥基嘧啶(1.11g,收率43%),為灰白色固體。其1H NMR(300MHz,DMSO-d6)數(shù)據(jù)如下:δ10.45(寬單峰,1H),8.67(單峰,1H),8.34(單峰,2H)。
參考文獻(xiàn):
[1] Chemistry - A European Journal, 2003, vol. 9, # 20, p. 4997 - 5010
[2] Patent: US2006/173049, 2006, A1. Location in patent: Page/Page column 28-29
[3] Patent: WO2008/65393, 2008, A1. Location in patent: Page/Page column 30
[4] Chemistry and Industry (London, United Kingdom), 1956, p. 1453
[5] Patent: US2002/143025, 2002, A1