952182-02-4

基本信息
1H-吡唑[3,4-B]吡啶-5-羧酸
1H-吡唑[3,4-B]吡啶-5-甲酸
1H-吡唑[3,4-B]嘧啶-5-羧酸
1H-吡唑并[3,4-B]吡啶-5-羧酸
1H-吡唑并[3,4-B]吡啶-5-甲酸
1H-PYRAZOLO[3,4-B]PYRIDINE-5-CARBOXYLIC ACID
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法
![1H-Pyrazolo[3,4-b]pyridine-5-carboxylic acid, 1-[(4-methoxyphenyl)methyl]-, ethyl ester](/CAS/20210111/GIF/1086423-59-7.gif)
1086423-59-7
![1H-吡唑并[3,4-B]吡啶-5-甲酸](/CAS/GIF/952182-02-4.gif)
952182-02-4
步驟5. 將1-(4-甲氧基芐基)-1H-吡唑并[3,4-b]吡啶-5-羧酸乙酯(4.4 g,14 mmol)溶解于三氟乙酸(TFA,158 mL)中,加熱至80℃。在80℃下持續(xù)攪拌反應(yīng)混合物4小時(shí)。反應(yīng)完成后,將混合物減壓濃縮至干。將殘余物小心倒入冰水中,隨后滴加2M氫氧化鈉(NaOH)水溶液調(diào)節(jié)pH至約14。通過(guò)過(guò)濾移除析出的固體,水相用乙酸乙酯洗滌。合并水相后,緩慢加入濃鹽酸(HCl)調(diào)節(jié)pH至中性(約7)。通過(guò)真空過(guò)濾收集析出的沉淀,并經(jīng)真空干燥,得到目標(biāo)產(chǎn)物1H-吡唑并[3,4-B]吡啶-5-甲酸,為白色固體(1 g,收率80%)。產(chǎn)物經(jīng)1H NMR(400 MHz,DMSO-d6)表征:δ 14.38-13.62(br,1H),9.07(d,J = 1.6 Hz,1H),8.81(d,J = 1.6 Hz,1H),8.32(s,1H)。質(zhì)譜(ESI+):m/z 164 [M+H]+。
參考文獻(xiàn):
[1] Patent: WO2013/127266, 2013, A1. Location in patent: Page/Page column 131; 133
[2] Patent: WO2013/127267, 2013, A1. Location in patent: Page/Page column 83; 84
[3] Patent: WO2013/127268, 2013, A1. Location in patent: Page/Page column 61; 62; 63
[4] Patent: WO2013/130935, 2013, A1. Location in patent: Paragraph 0182
[5] Patent: WO2013/130943, 2013, A1. Location in patent: Paragraph 0190