31402-54-7

基本信息
5-溴-2-甲基氨基嘧啶
5-溴-2-(甲氨基)嘧啶
5-溴-N-甲基-2-嘧啶胺
2-(N-甲基)-5-溴-嘧啶
5-Bromo-2-(methylamino)pyridine
5-BROMO-2-(METHYLAMINO)PYRIMIDINE
5-Bromo-N-methyl-2-pyrimidinamine
5-bromo-N-methylpyrimidin-2-amine
2-(Methylamino)-5-bromopyrimidine
(5-BROMOPYRIMIDIN-2-YL)METHYLAMINE
2-Pyrimidinamine, 5-bromo-N-methyl-
Pyrimidine, 5-bromo-2-(methylamino)-
N-(5-Bromopyrimidin-2-yl)-N-methylamine
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
常見問題列表

32779-36-5

74-89-5

31402-54-7
1. 在反應(yīng)瓶中加入5-溴-2-氯嘧啶(3g,15.5mmol)、40%甲胺水溶液(35ml)和甲醇(20ml),攪拌混合均勻。2. 將反應(yīng)混合物加熱至回流狀態(tài),保持反應(yīng)3天。3. 反應(yīng)完成后,冷卻至室溫。4. 使用旋轉(zhuǎn)蒸發(fā)儀在減壓條件下蒸發(fā)去除溶劑。5. 將殘余物用二氯甲烷和1M氫氧化鈉溶液進(jìn)行分配萃取。6. 分離有機(jī)層,并用無水硫酸鎂干燥。7. 過濾去除干燥劑后,再次使用旋轉(zhuǎn)蒸發(fā)儀在減壓條件下蒸發(fā)去除溶劑,得到白色固體產(chǎn)物5-溴-2-甲基氨基嘧啶(3.0g,收率100%)。8. 產(chǎn)物經(jīng)1H-NMR(CDCl3)表征:δ 2.98(3H,d,J=5.12Hz),5.16(1H,brs),8.29(2H,s)。
參考文獻(xiàn):
[1] Patent: US2010/130492, 2010, A1. Location in patent: Page/Page column 93
[2] Patent: WO2010/12747, 2010, A1. Location in patent: Page/Page column 16-17
[3] Patent: WO2007/84786, 2007, A1. Location in patent: Page/Page column 90
[4] ACS Medicinal Chemistry Letters, 2011, vol. 2, # 1, p. 34 - 38
[5] Patent: WO2012/109423, 2012, A1. Location in patent: Page/Page column 18