3-(3-异丙基-5-甲基-4H-1,2,4-三唑-4-基)-8-氮杂双环[3.2.1]]辛烷对甲苯磺酸盐合成路线 (共 8 条)
反应条件
sodium tris(acetoxy)borohydride; acetic acid in 1,2-dichloro-ethane T=0 - 20°C; 3 h; Inert atmosphere;
参考文献
Asano, Shigehiro; Gavrilyuk, Julia; Burton, Dennis R.; Barbas, Carlos F.
ACS Medicinal Chemistry Letters, 2014 , vol. 5, # 2 p. 133 - 137
反应条件
sodium tris(acetoxy)borohydride in ethyl acetate T=0 - 15°C; 2 h; Inert atmosphereLarge scale;
参考文献
Ahman, Jens; Birch, Melissa; Haycock-Lewandowski, Sarah J.; Long, James; Wilder, Alexander
Organic Process Research and Development, 2008 , vol. 12, # 6 p. 1104 - 1113
反应条件
5 palladium on charcoal; hydrogen in methanol
T=50°C; P=2250.23 Torr; Inert atmosphereLarge scale; SolventTime;
参考文献
Ahman, Jens; Birch, Melissa; Haycock-Lewandowski, Sarah J.; Long, James; Wilder, Alexander
Organic Process Research and Development, 2008 , vol. 12, # 6 p. 1104 - 1113
反应条件
1: sodium; propan-1-ol / toluene / 12 h / |Reflux; |Inert atmosphere
2: tetrahydrofuran / 72 h / 20 °C / |Inert atmosphere
3: hydrogenchloride / methanol; 1,4-dioxane / 2 h / 20 °C / |Inert atmosphere
4: sodium carbonate / water; dichloromethane / 0 - 20 °C / |Inert atmosphere
5: phosphorus pentachloride / dichloromethane / 2 h / 0 - 20 °C / |Inert atmosphere
6: dichloromethane; 1,1-dimethylpropan-1-ol / 0 - 20 °C / |Inert atmosphere
7: acetic acid / ethyl acetate / 0.5 h / 80 °C / |Inert atmosphere
8: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2585.81 Torr / |Inert atmosphere
View Scheme
参考文献
Asano, Shigehiro; Gavrilyuk, Julia; Burton, Dennis R.; Barbas, Carlos F.
ACS Medicinal Chemistry Letters, 2014 , vol. 5, # 2 p. 133 - 137
反应条件
1: hydrogenchloride / methanol; 1,4-dioxane / 2 h / 20 °C / |Inert atmosphere
2: sodium carbonate / water; dichloromethane / 0 - 20 °C / |Inert atmosphere
3: phosphorus pentachloride / dichloromethane / 2 h / 0 - 20 °C / |Inert atmosphere
4: dichloromethane; 1,1-dimethylpropan-1-ol / 0 - 20 °C / |Inert atmosphere
5: acetic acid / ethyl acetate / 0.5 h / 80 °C / |Inert atmosphere
6: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2585.81 Torr / |Inert atmosphere
View Scheme
参考文献
Asano, Shigehiro; Gavrilyuk, Julia; Burton, Dennis R.; Barbas, Carlos F.
ACS Medicinal Chemistry Letters, 2014 , vol. 5, # 2 p. 133 - 137
反应条件
1: sodium carbonate / water; dichloromethane / 0 - 20 °C / |Inert atmosphere
2: phosphorus pentachloride / dichloromethane / 2 h / 0 - 20 °C / |Inert atmosphere
3: dichloromethane; 1,1-dimethylpropan-1-ol / 0 - 20 °C / |Inert atmosphere
4: acetic acid / ethyl acetate / 0.5 h / 80 °C / |Inert atmosphere
5: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2585.81 Torr / |Inert atmosphere
View Scheme
参考文献
Asano, Shigehiro; Gavrilyuk, Julia; Burton, Dennis R.; Barbas, Carlos F.
ACS Medicinal Chemistry Letters, 2014 , vol. 5, # 2 p. 133 - 137
反应条件
1: phosphorus pentachloride / dichloromethane / 2 h / 0 - 20 °C / |Inert atmosphere
2: dichloromethane; 1,1-dimethylpropan-1-ol / 0 - 20 °C / |Inert atmosphere
3: acetic acid / ethyl acetate / 0.5 h / 80 °C / |Inert atmosphere
4: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2585.81 Torr / |Inert atmosphere
View Scheme
参考文献
Asano, Shigehiro; Gavrilyuk, Julia; Burton, Dennis R.; Barbas, Carlos F.
ACS Medicinal Chemistry Letters, 2014 , vol. 5, # 2 p. 133 - 137
反应条件
1: hydroxylamine hydrochloride; sodium hydroxide / ethanol; water / 20 h / |Inert atmosphere; |Reflux
2: sodium; propan-1-ol / toluene / 12 h / |Reflux; |Inert atmosphere
3: tetrahydrofuran / 72 h / 20 °C / |Inert atmosphere
4: hydrogenchloride / methanol; 1,4-dioxane / 2 h / 20 °C / |Inert atmosphere
5: sodium carbonate / water; dichloromethane / 0 - 20 °C / |Inert atmosphere
6: phosphorus pentachloride / dichloromethane / 2 h / 0 - 20 °C / |Inert atmosphere
7: dichloromethane; 1,1-dimethylpropan-1-ol / 0 - 20 °C / |Inert atmosphere
8: acetic acid / ethyl acetate / 0.5 h / 80 °C / |Inert atmosphere
9: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2585.81 Torr / |Inert atmosphere
View Scheme
参考文献
Asano, Shigehiro; Gavrilyuk, Julia; Burton, Dennis R.; Barbas, Carlos F.
ACS Medicinal Chemistry Letters, 2014 , vol. 5, # 2 p. 133 - 137