24638-29-7

基本信息
2,3-二氨基-5-甲基吡啶
5-甲基-2,3-二氨基吡啶
2,3-Diamino-5-methylpyridine
5-Methyl-2,3-diaMinopyridine
5-Methyl-2,3-pyridinediamine
3-Picoline,5,6-diamino- (8CI)
2,3-Pyridinediamine, 5-methyl-
2,3-Diamino-5-methylpyridine ISO 9001:2015 REACH
制備方法

7598-26-7

24638-29-7
以2-氨基-3-硝基-5-甲基吡啶為原料合成2,3-二氨基-5-甲基吡啶的一般步驟如下:將Pd/C催化劑(50 mg,0.47 mmol)加入攪拌中的2-氨基-5-甲基-3-硝基吡啶(500 mg,3.27 mmol)的甲醇(7 mL)溶液中。隨后,對(duì)反應(yīng)體系進(jìn)行三次抽真空并充入氫氣置換。在氫氣氛圍下,于20℃攪拌反應(yīng)5小時(shí)。反應(yīng)完成后,通過(guò)硅藻土過(guò)濾反應(yīng)混合物,并用額外的甲醇(30 mL)洗滌濾餅。將濾液在減壓下濃縮,得到目標(biāo)產(chǎn)物2,3-二氨基-5-甲基吡啶(395 mg,收率98%)。產(chǎn)物經(jīng)1H NMR(MeOD)表征:δ 7.22(dd,J = 2.0, 0.9 Hz,1H),6.81(dd,J = 2.0, 0.7 Hz,1H),2.13(t,J = 0.7 Hz,3H)。質(zhì)譜分析顯示m/z = 124(100)。
參考文獻(xiàn):
[1] Journal of Medicinal Chemistry, 1997, vol. 40, # 22, p. 3679 - 3686
[2] Patent: WO2017/219083, 2017, A1. Location in patent: Page/Page column 73; 74
[3] Patent: US2014/315888, 2014, A1. Location in patent: Paragraph 0754-0755
[4] Journal of the American Chemical Society, 1950, vol. 72, p. 2806
[5] Patent: US5620978, 1997, A