473927-64-9
473927-64-9 結(jié)構(gòu)式
基本信息
(4-碘苯基)-1-(4-甲氧基苯基)-7-氧代-4,5,6,7-四氫-1H-吡
6-(4-碘苯基)-1-(4-甲氧基苯基)-7-氧代-4,5,6,7-四氫-1H-吡唑并[3,4-C]吡啶-3-羧酸
6-(4-碘苯基)-1-(4-甲氧基苯基)-7-氧代-4,5,6,7-四氫-1H-吡唑并[3,4-C]吡啶-3-羧酸乙酯
6-(4-碘苯基)-1-(4-甲氧基苯基)-7-氧代-4,5,6,7-四氫-1H-吡唑并[3,4-C]吡啶-3-羧酸乙酯,阿哌沙班中間體
6-(4-碘苯基)-1-(4-甲氧基苯基)-7-氧代-4,5,6,7-四氫-1H-吡唑并[3,4-C]吡啶-3-羧酸乙酯,阿哌沙班中間體 10G
Apixaban Impurity 107
AXN-IIIQ: What is AXN-III Q: What is the CAS Number of AXN-III
Ethyl 6-(4-iodophenyl)-1-(4-methoxyphenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine
ethyl 6-(4-iodophenyl)-1-(4-methoxyphenyl)-7-oxo-4,5-dihydropyrazolo[3,4-c]pyridine-3-carboxylate
Ethyl 6-(4-iodophenyl)-1-(4-methoxyphenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-
1-(4-Methoxyphenyl)-6-(4-iodophenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxyli
6-(4-iodophenyl)-1-(4-Methoxyphenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylate
Ethyl 6-(4-iodophenyl)-1-(4-methoxyphenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylate
1-(4-Methoxyphenyl)-6-(4-iodophenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylic acid ethyl este
物理化學(xué)性質(zhì)
制備方法
473927-69-4
![[(4-甲氧基苯基)肼基]氯乙酸乙酯](/CAS2/GIF/27143-07-3.gif)
27143-07-3
473927-64-9
在惰性氣氛（氬氣）下進行反應(yīng)。首先，將[(4-甲氧基苯基)亞肼基]氯乙酸乙酯（14.1 g, 0.055 mol）溶解于140 mL乙酸乙酯中。將溶液置于冰水浴中冷卻至0-5℃。在攪拌條件下，分批加入1-(4-碘苯基)-3-嗎啉-5,6-二氫吡啶-2(1H)-酮（21.1 g, 0.055 mol）。隨后，在0-5℃下緩慢滴加三乙胺（11.1 g, 0.110 mol）。停止冷卻，讓反應(yīng)混合物升溫至室溫。接著，加熱反應(yīng)混合物至回流狀態(tài)，并維持回流約1小時。反應(yīng)進程通過HPLC監(jiān)測，確保反應(yīng)在120分鐘內(nèi)完成。再次將反應(yīng)混合物冷卻至0-5℃，緩慢滴加由濃鹽酸（27.5 mL, 0.275 mol）與等體積蒸餾水稀釋的1:1鹽酸溶液。冷卻后，繼續(xù)攪拌反應(yīng)混合物約1小時。然后，加入55 mL水，將形成的懸浮液在冷卻條件下繼續(xù)攪拌2小時。通過過濾分離產(chǎn)物，并在50℃下真空干燥24小時，得到6-(4-碘苯基)-1-(4-甲氧基苯基)-7-氧代-4,5,6,7-四氫-1H-吡唑并[3,4-c]吡啶-3-羧酸（產(chǎn)物III），產(chǎn)量21.3 g，產(chǎn)率75%，HPLC純度為95%。
參考文獻：
[1] Patent: WO2014/75648, 2014, A1. Location in patent: Page/Page column 11
[2] Patent: WO2015/177801, 2015, A1. Location in patent: Page/Page column 23