356068-93-4

基本信息
蘇尼替尼中間體
舒尼替尼中間體7
舒尼替尼雜質(zhì)34
蘋(píng)果酸舒尼替尼雜質(zhì)C
蘋(píng)果酸舒尼替尼中間體3
5-((Z)-(5-氟-2-氧代吲哚烷-3-亞基)甲基)
5-((Z)-(5-氟-2-吲哚酮-3-基)甲基)-2,4-二甲基吡咯-3-羧酸
5-((Z)-(5-氟-2-氧代吲哚烷-3-亞基)甲基)-2,4-二甲基-1H-吡咯
(Z)-2,4-二甲基-5-[(2-氧代-5-氟吲哚啉-3-亞基)甲基]吡咯-3-甲酸
5-((Z)-(5-Fluoro-2-oxoindolin-3-ylidene)methyl)-2,4-dimethyl...
(Z)-5-[(5-Fluoro-2-oxoindolin-3-ylidene)methyl]-2,4-dimethylpyrrole-3-carboxylic Acid
(Z)-5-((5-fluoro-2-oxoindolin-3-ylidene)Methyl)-2,4-diMethyl-1H-pyrrole-3-carboxylic acid
5-((Z)-(5-Fluoro-2-oxoindolin-3-ylidene)methyl)-2,4-dimethyl-1H-pyrrole-3-carboxylic acid
(3Z)-3-[(3,5-Dimethyl-4-carboxy-1H-pyrrol-2-yl)methylidene]-5-fluoro-1,3-dihydro-2H-indol-2-on
(3Z)-3-[(3,5-DiMethyl-4-carboxy-1H-pyrrol-2-yl)Methylidene]-5-fluoro-1,3-dihydro-2H-indol-2-one
1H-Pyrrole-3-carboxylic acid, 5-[(Z)-(5-fluoro-1,2-dihydro-2-oxo-3H-indol-3-ylidene)methyl]-2,4-dimethyl-
物理化學(xué)性質(zhì)
制備方法

253870-02-9

56341-41-4

356068-93-4
以2,4-二甲基-5-醛基-1H-吡咯-3-羧酸(8,1.0g,6.61mmol)和5-氟吲哚-2-酮(14,1.1g,3.77mmol)為原料,在室溫下將硫酸銨((NH4)2SO4,0.09g,0.67mmol)加入至六甲基二硅氮烷(HMDS,20mL)中的攪拌混合物中。隨后,將反應(yīng)混合物加熱至回流并維持該溫度至少5小時(shí),反應(yīng)進(jìn)程通過(guò)氣相色譜(GC)監(jiān)測(cè)。反應(yīng)完成后,加入5-氟吲哚-2-酮(14)和三氟甲磺酸三甲基硅酯(TMSOTf,0.29g,1.32mmol)。繼續(xù)攪拌混合物,直至高效液相色譜(HPLC)分析顯示反應(yīng)完成。反應(yīng)混合物用水(6mL)和乙腈(MeCN,30mL)淬滅,過(guò)濾后,濾餅依次用乙腈(20mL)和乙醇(EtOH,5mL)洗滌。最后,將產(chǎn)物在40℃下真空干燥過(guò)夜,得到目標(biāo)化合物5-((Z)-(5-氟-2-氧代吲哚烷-3-亞基)甲基)-2,4-二甲基-1H-吡咯-3-羧酸(15,1.92g,收率97%),為黃色至棕色粉末,HPLC純度約為82.1%。
參考文獻(xiàn):
[1] Patent: US2013/190512, 2013, A1. Location in patent: Paragraph 0088
[2] Patent: WO2007/81560, 2007, A2. Location in patent: Page/Page column 6
[3] Patent: WO2006/127961, 2006, A1. Location in patent: Page/Page column 15-16
[4] Patent: WO2008/33562, 2008, A2. Location in patent: Page/Page column 34
[5] Patent: US2009/76005, 2009, A1. Location in patent: Page/Page column 12; 13