147269-67-8

基本信息
芐基(2-氧代-1,2-二氫吡啶-3-基)氨基甲酸酯
BENZYL 2-OXO-1,2-DIHYDROPYRIDIN-3-YLCARBAMATE
benzyl N-(2-oxo-1,2-dihydropyridin-3-yl)carbaMate
(2-Oxo-1,2-dihydropyridin-3-yl)carbamic acid benzyl ester
BENZYL 2-OXO-1,2-DIHYDROPYRIDIN-3-YLCARBAMATE ISO 9001:2015 REACH
Carbamic acid, N-(1,2-dihydro-2-oxo-3-pyridinyl)-, phenylmethyl ester
物理化學(xué)性質(zhì)
制備方法

33630-99-8

501-53-1

147269-67-8
在室溫下,將3-氨基吡啶-2(1H)-酮(3.25 g,29.5 mmol)和碳酸鈉(6.26 g,59.0 mmol)溶于四氫呋喃(100 mL)中,緩慢滴加氯甲酸芐酯(5.27 mL,36.9 mmol)。反應(yīng)混合物在室溫下攪拌24小時(shí)。反應(yīng)完成后,用乙酸乙酯(150 mL)稀釋反應(yīng)混合物,并通過Celite過濾。濾液在減壓下濃縮至約200 mL,隨后用水(40 mL)洗滌,并用無水硫酸鎂干燥。再次減壓濃縮至約50 mL,通過抽濾收集析出的白色固體(第一批產(chǎn)物)。將剩余濾液減壓濃縮至近干,殘余物與乙醚(50 mL)攪拌,通過抽濾收集不溶的白色固體(第二批產(chǎn)物)。合并兩批產(chǎn)物,在50℃下真空干燥,得到目標(biāo)化合物(2-氧代-1,2-二氫吡啶-3-基)氨基甲酸芐酯(5.77 g,23.62 mmol,產(chǎn)率80%),為白色固體。
參考文獻(xiàn):
[1] ChemMedChem, 2011, vol. 6, # 7, p. 1228 - 1237
[2] Patent: WO2007/27729, 2007, A1. Location in patent: Page/Page column 39-40
[3] Patent: WO2015/89143, 2015, A1. Location in patent: Page/Page column 83; 84
[4] Journal of Medicinal Chemistry, 1994, vol. 37, # 19, p. 3090 - 3099
[5] Patent: US2007/287696, 2007, A1. Location in patent: Page/Page column 33