2,5-吡啶二甲酸二乙酯合成路线 （共 18 条）
反应条件
1: 3-chloro-benzenecarboperoxoic acid / dichloromethane / 24 h / 20 °C 2: hydrogenchloride; water / ethanol / 14.5 h / 60 °C 3: N,N-dimethyl-formamide; thionyl chloride / dichloromethane / 2.5 h / 65 °C / Cooling with ice View Scheme
参考文献
Shionogi and Co., Ltd.
Patent: EP2305672 A1, 2011 ;
反应条件
1: sodium tetrahydroborate / ethanol / 14 h / Reflux 2: thionyl chloride / toluene / 20 °C 3: lithium aluminium tetrahydride / tetrahydrofuran / 1 h / 0 °C 4: 1-hydroxy-3H-benz[d][1,2]iodoxole-1,3-dione / dimethyl sulfoxide / 2 h / 20 °C View Scheme
参考文献
Journal of Porphyrins and Phthalocyanines, , vol. 14, # 6 p. 469 - 480
反应条件
1.1: calcium chloride; sodium tetrahydroborate / ethanol / 0.75 h / -5 °C
2.1: triethylamine; methanesulfonyl chloride / dichloromethane / 0 °C
2.2: 60 °C
3.1: triphenylphosphine / tetrahydrofuran / 60 °C
4.1: acetic anhydride / 0.5 h / 50 °C
4.2: 20 °C
5.1: trichlorophosphate / toluene / Reflux
View Scheme
参考文献
ShionogiandCo., Ltd.
Patent: EP2341053 A1, 2011 ;
反应条件
1: 51 percent / NaBH4, CaCl2 / ethanol / 16 h / Ambient temperature
2: 59 percent / SeO2, H2O / dioxane / 3 h / 100 °C
3: 97 percent / 30percent H2O2 / H2O / 16 h / Ambient temperature
4: 1.) Et3N, CaCl2, 2.) H2SO4 / 1.) EtOH, 2.) reflux, 4 h
View Scheme
参考文献
Dawson, Marcia I.; Chan, Rebecca; Hobbs, Peter D.; Chao, Wan-ru; Schiff, Leonard J.
Journal of Medicinal Chemistry, 1983 , vol. 26, # 9 p. 1282 - 1293
反应条件
ethanol; hydrazine hydrate
参考文献
Shinohara et al.
Kobunshi Kagaku, 1958 , vol. 15, p. 839,844
Chem.Abstr., 1960 , p. 22636
反应条件
1: 67 percent / NaBH4, CaCl2 / ethanol / 16 h / Ambient temperature
2: HBr / acetic acid / 144 h / Ambient temperature
3: 62 percent / t-BuOK, Cs2CO3 / aq. ethanol / 16 h / Heating
4: 84 percent / P(OMe)3 / 18 h / Ambient temperature; Irradiation
View Scheme
参考文献
Woersdoerfer, Udo; Voegtle, Fritz; Nieger, Martin; Waletzke, Mirko; Grimme, Stefan; Glorius, Frank; Pfaltz, Andreas
Synthesis, 1999 , # 4 p. 597 - 602
反应条件
1: 51 percent / NaBH4, CaCl2 / ethanol / 16 h / Ambient temperature
2: 59 percent / SeO2, H2O / dioxane / 3 h / 100 °C
3: 97 percent / 30percent H2O2 / H2O / 16 h / Ambient temperature
4: 1.) Et3N, CaCl2, 2.) H2SO4 / 1.) EtOH, 2.) reflux, 4 h
5: 59 percent / CrO3, pyridine / CH2Cl2 / 4 h / Ambient temperature
View Scheme
参考文献
Dawson, Marcia I.; Chan, Rebecca; Hobbs, Peter D.; Chao, Wan-ru; Schiff, Leonard J.
Journal of Medicinal Chemistry, 1983 , vol. 26, # 9 p. 1282 - 1293
反应条件
1: 51 percent / NaBH4, CaCl2 / ethanol / 16 h / Ambient temperature
2: 59 percent / SeO2, H2O / dioxane / 3 h / 100 °C
3: 97 percent / 30percent H2O2 / H2O / 16 h / Ambient temperature
View Scheme
参考文献
Dawson, Marcia I.; Chan, Rebecca; Hobbs, Peter D.; Chao, Wan-ru; Schiff, Leonard J.
Journal of Medicinal Chemistry, 1983 , vol. 26, # 9 p. 1282 - 1293
