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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
59608-03-6
合成路线
(共 10 条)
6283-81-4
3-氧代-3-(3-吡啶基)丙酸乙酯
→
反应条件
59608-03-6
反应条件
trifluoromethylsulfonic anhydride; triethylamine; triphenyl-phosphine oxide in 1,2-dichloro-ethane T=85°C; 2 h; Inert atmosphere;
参考文献
GLAXO GROUP LIMITED; JOHNS, Brian Alvin; SHOTWELL, John Brad
Patent: WO2012/67664 A1, 2012 ;
Location in patent: Page/Page column 29 ;
2510-23-8
3-乙炔基吡啶
+
64-17-5
乙醇
+
201230-82-2
→
反应条件
59608-03-6
反应条件
palladium 10 on activated carbon; oxygen; tetra-(n-butyl)ammonium iodide in 1,4-dioxane T=80°C; P=760.051 Torr; 8 h; Autoclave;
参考文献
Gadge, Sandip T.; Bhanage, Bhalchandra M.
Synlett, 2013 , vol. 24, # 8 art. no. ST-2013-D0181-L, p. 981 - 986
1120-90-7
3-碘吡啶
+
143952-57-2
→
反应条件
59608-03-6
反应条件
tetraethylammonium chloride; bis-triphenylphosphine-palladium(II) chloride in tetrahydrofuran T=50°C; 3 h;
参考文献
Sakamoto; Shiga; Yasuhara; Uchiyama; Kondo; Yamanaka
Synthesis, 1992 , # 8 p. 746 - 748
1120-90-7
3-碘吡啶
+
16205-84-8
3-(三甲基甲硅烷基)丙酸乙酯
→
反应条件
59608-03-6
反应条件
AgCl; tetrakis(triphenylphosphine) palladium(0) in N,N-dimethyl-formamide T=20°C; 12 h;
参考文献
Lecercle, Delphine; Mothes, Celine; Taran, Frederic
Synthetic Communications, 2007 , vol. 37, # 8 p. 1301 - 1311
1120-90-7
3-碘吡啶
→
反应条件
59608-03-6
反应条件
bis-triphenylphosphine-palladium(II) chloride in tetrahydrofuran; hexane T=50°C; 2 h;
参考文献
Sakamoto; Shiga; Yasuhara; Uchiyama; Kondo; Yamanaka
Synthesis, 1992 , # 8 p. 746 - 748
500-22-1
3-吡啶甲醛
+
623-49-4
氰基甲酸乙酯
→
反应条件
59608-03-6
反应条件
1: pyridine-3-aldehyde With TMSC(Li)N2 in tetrahydrofuran; hexane T=-78 - 20°C; 1.5 h; 2: With n-butyllithium in tetrahydrofuran; hexane T=-78°C; 0.5 h; 3: [(Cyanocarbonyl)oxy]ethane in tetrahydrofuran; hexane T=-78°C; 0.5 h; Further stages.;
参考文献
Hari, Yoshiyuki; Date, Koji; Aoyama, Toyohiko
Heterocycles, 2007 , vol. 74, # C p. 545 - 552
1120-90-7
3-碘吡啶
→
反应条件
59608-03-6
反应条件
1: Et3N / (PPh3)2PdCl2, CuI / 4 h / Ambient temperature 2: p-toluenesulfonic acid / benzene / 12 h / Ambient temperature View Scheme
参考文献
Sakamoto; Shiga; Yasuhara; Uchiyama; Kondo; Yamanaka
Synthesis, 1992 , # 8 p. 746 - 748
42217-00-5
→
反应条件
59608-03-6
反应条件
1: Et3N / (PPh3)2PdCl2, CuI / 4 h / Ambient temperature 2: p-toluenesulfonic acid / benzene / 12 h / Ambient temperature View Scheme
参考文献
Sakamoto; Shiga; Yasuhara; Uchiyama; Kondo; Yamanaka
Synthesis, 1992 , # 8 p. 746 - 748
59-67-6
烟酸
→
反应条件
59608-03-6
反应条件
1.1: oxalyl dichloride / N,N-dimethyl-formamide / dichloromethane / 1.5 h / Reflux 2.1: triethylamine; magnesium chloride / acetonitrile / 2 h / Cooling with ice-salt bath 2.2: 20 °C / Cooling with ice-salt bath 2.3: 1.5 h / Cooling with ice 3.1: trifluoromethylsulfonic anhydride; triethylamine; triphenyl-phosphine oxide / 1,2-dichloro-ethane / 2 h / 85 °C / Inert atmosphere View Scheme
参考文献
GLAXO GROUP LIMITED; JOHNS, Brian Alvin; SHOTWELL, John Brad
Patent: WO2012/67664 A1, 2012 ;
10400-19-8
吡啶-3-羧酸酰氯
→
反应条件
59608-03-6
反应条件
1.1: triethylamine; magnesium chloride / acetonitrile / 2 h / Cooling with ice-salt bath 1.2: 20 °C / Cooling with ice-salt bath 1.3: 1.5 h / Cooling with ice 2.1: trifluoromethylsulfonic anhydride; triethylamine; triphenyl-phosphine oxide / 1,2-dichloro-ethane / 2 h / 85 °C / Inert atmosphere View Scheme
参考文献
GLAXO GROUP LIMITED; JOHNS, Brian Alvin; SHOTWELL, John Brad
Patent: WO2012/67664 A1, 2012 ;