771579-27-2

基本信息
3-(氨基甲基)-4,6-二甲基-1,2-二氫吡啶-2-酮
3-(氨基甲基)-4,6-二甲基-2(1H)-吡啶酮(9CI)
3-(aminomethyl)-4,6-dimethyl-1H-pyridin-2-one
3-(Aminomethyl)-4,6-dimethyl-2(1H)-pyridinone
2(1H)-Pyridinone,3-(aMinoMethyl)-4,6-diMethyl-
2(1H)-Pyridinone, 3-(aminomethyl)-4,6-dimethyl- (9CI)
3-(AMinoMethyl)-4,6-diMethyl-1,2-dihydropyridin-2-one
3-(AMinoMethyl)-4,6-diMethyl-1,2-dihydropyridine-2-one
3-(Aminomethyl)-4,6-Dimethylpyridin-2(1H)-One(WX603161)
(4,6-dimethyl-2-oxo-1H-pyridin-3-yl)methylazanium chloride
2(1H)-Pyridinone,3-(aMinoMethyl)-4,6-diMethyl-,hydrochloride(1:1)
物理化學(xué)性質(zhì)
制備方法

769-28-8

771579-27-2
以2-氧代-4,6-二甲基-1,2-二氫吡啶-3-甲腈為原料合成3-(氨甲基)-4,6-二甲基吡啶-2(1H)-酮的一般步驟:將碳載鈀(10%,324 mg)和氧化鉑(21.8 mg)加入到4,6-二甲基-2-氧代-1,2-二氫吡啶-3-甲腈(3 g,20.3 mmol)的混合物中,加入乙酸鈉(3.1 g,37.5 mmol)和乙酸(100 mL)。將反應(yīng)混合物在氫氣氣氛下攪拌48小時。反應(yīng)完成后,通過硅藻土墊過濾反應(yīng)混合物,濾液濃縮至干。將殘余物用濃鹽酸(3 mL)和乙醇(15 mL)處理,冷卻至0℃并在該溫度下攪拌2小時,形成懸浮液。通過抽濾收集沉淀,依次用冷乙醇和乙醚洗滌,真空干燥,得到白色固體產(chǎn)物(3.5 g,收率92%),熔點(diǎn)為253-258℃。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(400 MHz, DMSO-d6)和13C NMR(100 MHz, DMSO-d6)確認(rèn),并進(jìn)行了高分辨質(zhì)譜(HRMS-ESI)分析,結(jié)果與預(yù)期一致。
參考文獻(xiàn):
[1] Synthetic Communications, 2016, vol. 46, # 14, p. 1215 - 1222
[2] Patent: WO2013/75083, 2013, A1. Location in patent: Paragraph 00177; 00178
[3] Patent: US9206128, 2015, B2. Location in patent: Page/Page column 103; 104
[4] ACS Medicinal Chemistry Letters, 2012, vol. 3, # 12, p. 1091 - 1096
[5] Journal of Medicinal Chemistry, 2016, vol. 59, # 16, p. 7617 - 7633