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结构式
乙二醇
甲醛
63148-62-9
MDI
丁酮
二甲基亚砜
碳酸氢钠
471-34-1
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乙二醇
甲醛
63148-62-9
MDI
丁酮
二甲基亚砜
碳酸氢钠
471-34-1
吉非替尼中间体B
合成路线
(共 16 条)
788136-89-0
4-(3-氯-4-氟苯氨基)-7-甲氧基喹唑啉-6-醇乙酸酯
→
反应条件
912556-91-3
吉非替尼中间体B
反应条件
1: water; sodium hydroxide / methanol / 6 h / 20 °C 2: potassium carbonate; potassium iodide / N,N-dimethyl-formamide / 6 h / 40 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Jiancun; ZHANG, Yingjun; ZHANG, Weihong; LIU, Bing; ZHANG, Jiquan; LIU, Jinlei; ZHANG, Lu
Patent: WO2013/71697 A1, 2013 ;
13794-72-4
6,7-二甲氧基喹唑啉-4-酮
→
反应条件
912556-91-3
吉非替尼中间体B
反应条件
1.1: methanesulfonic acid; dl-methionine / 3 h / 130 °C / |Cooling with ice 1.2: pH 7 2.1: pyridine / 3 h / 20 - 100 °C 3.1: thionyl chloride / N,N-dimethyl-formamide / 3 h / 70 °C 4.1: isopropyl alcohol / 5 h / 88 °C 5.1: water; sodium hydroxide / methanol / 6 h / 20 °C 6.1: potassium carbonate; potassium iodide / N,N-dimethyl-formamide / 6 h / 40 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Jiancun; ZHANG, Yingjun; ZHANG, Weihong; LIU, Bing; ZHANG, Jiquan; LIU, Jinlei; ZHANG, Lu
Patent: WO2013/71697 A1, 2013 ;
5653-40-7
2-氨基-4,5-二甲氧基苯甲酸
→
反应条件
912556-91-3
吉非替尼中间体B
反应条件
1.1: trimethyl orthoformate / methanol / 4 h / 70 °C / |Reflux 2.1: methanesulfonic acid; dl-methionine / 3 h / 130 °C / |Cooling with ice 2.2: pH 7 3.1: pyridine / 3 h / 20 - 100 °C 4.1: thionyl chloride / N,N-dimethyl-formamide / 3 h / 70 °C 5.1: isopropyl alcohol / 5 h / 88 °C 6.1: water; sodium hydroxide / methanol / 6 h / 20 °C 7.1: potassium carbonate; potassium iodide / N,N-dimethyl-formamide / 6 h / 40 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Jiancun; ZHANG, Yingjun; ZHANG, Weihong; LIU, Bing; ZHANG, Jiquan; LIU, Jinlei; ZHANG, Lu
Patent: WO2013/71697 A1, 2013 ;
179688-52-9
6-羟基-7-甲氧基-3H-喹唑啉-4-酮
→
反应条件
912556-91-3
吉非替尼中间体B
反应条件
1: pyridine / 3 h / 20 - 100 °C 2: thionyl chloride / N,N-dimethyl-formamide / 3 h / 70 °C 3: isopropyl alcohol / 5 h / 88 °C 4: water; sodium hydroxide / methanol / 6 h / 20 °C 5: potassium carbonate; potassium iodide / N,N-dimethyl-formamide / 6 h / 40 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Jiancun; ZHANG, Yingjun; ZHANG, Weihong; LIU, Bing; ZHANG, Jiquan; LIU, Jinlei; ZHANG, Lu
Patent: WO2013/71697 A1, 2013 ;
621-59-0
3-羟基-4-甲氧基苯甲醛
→
反应条件
912556-91-3
吉非替尼中间体B
反应条件
1: potassium carbonate / 60 °C 2: potassium permanganate / acetone / |Reflux 3: thionyl chloride / |Reflux 4: acetic anhydride; acetic acid; nitric acid / 0 - 5 °C 5: acetic acid; iron / methanol 6: ethanol / |Reflux 7: trichlorophosphate; triethylamine / toluene / |Reflux 8: isopropyl alcohol / |Reflux View Scheme
参考文献
Zhao, Feng; Lin, Zhaohu; Wang, Feng; Zhao, Weili; Dong, Xiaochun
Bioorganic and Medicinal Chemistry Letters, 2013 , vol. 23, # 19 p. 5385 - 5388
929683-54-5
→
反应条件
912556-91-3
吉非替尼中间体B
反应条件
1: potassium permanganate / acetone / |Reflux 2: thionyl chloride / |Reflux 3: acetic anhydride; acetic acid; nitric acid / 0 - 5 °C 4: acetic acid; iron / methanol 5: ethanol / |Reflux 6: trichlorophosphate; triethylamine / toluene / |Reflux 7: isopropyl alcohol / |Reflux View Scheme
参考文献
Zhao, Feng; Lin, Zhaohu; Wang, Feng; Zhao, Weili; Dong, Xiaochun
Bioorganic and Medicinal Chemistry Letters, 2013 , vol. 23, # 19 p. 5385 - 5388
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