7400-06-8
7400-06-8 結(jié)構(gòu)式
基本信息
6-氨基-5-(2,2-二乙氧基乙基)-4-羥基嘧啶
6-氨基-5-(2,2-二乙氧基乙基)嘧啶-4(3H)-酮
6-氨基-5-(2,2-二乙氧基乙基)-4(3H)-嘧啶酮
Tofacitinib Impurity 203
6-Amino-5-(2,2-diethoxyethyl)
6-Amino-5-(2,2-diethoxyethyl)pyrimidin-4-ol
6-amino-5-(2,2-diethoxyethyl)-1H-pyrimidin-4-one
6-AMino-5-(2,2-diethoxyethyl)-4(3H)-pyriMidinone
6-aMino-5-(2,2-diethoxyethyl)pyriMidin-4(3H)-one
4(3H)-PyriMidinone, 6-aMino-5-(2,2-diethoxyethyl)-
6-aMino-5-(2,2-diethoxyethyl)-1,4-dihydropyriMidin-4- one
物理化學(xué)性質(zhì)
制備方法
7400-05-7
7400-06-8
步驟i: 將6-氨基-5-(2,2-二乙氧基乙基)-2-巰基-4-羥基嘧啶（11.6 mmol）[制備方法參見Davoll, J., J. Chem. Soc., 1960, pp131-138]溶解于水（150 mL）和氨水溶液（9 mL）的混合溶劑中，加熱至90℃。向反應(yīng)混合物中分批加入Raney Nickel懸浮液（每次2-3 mL），直至TLC和LC/MS分析顯示反應(yīng)完成。將反應(yīng)混合物冷卻至室溫，通過硅藻土墊過濾，濾餅用水洗滌（2×25 mL）。合并的水相濾液經(jīng)冷凍干燥，得到6-氨基-5-(2,2-二乙氧基乙基)-4-羥基嘧啶，為灰白色粉末，產(chǎn)量2.23 g（85%）。LC/MS: RT = 1.37 min; m/z = 182 [M-EtOH + H]+?？傔\(yùn)行時(shí)間為3.75 min。1H NMR (DMSO-d6): δ 1.07 (t, 6H); 3.40 (m, 2H); 3.59 (m, 2H); 4.56 (t, 1H); 6.07 (br s, 2H); 7.70 (s, 1H); 11.43 (br s, 1H)。
參考文獻(xiàn)：
[1] Patent: WO2007/104944, 2007, A1. Location in patent: Page/Page column 43
[2] Patent: WO2006/46023, 2006, A1. Location in patent: Page/Page column 123
[3] Patent: WO2008/75109, 2008, A1. Location in patent: Page/Page column 112
[4] Patent: WO2006/46024, 2006, A1. Location in patent: Page/Page column 118
[5] Patent: WO2007/125321, 2007, A2. Location in patent: Page/Page column 116