2,4-二哌啶酮-1-甲酸叔丁酯合成路线 (共 15 条)
反应条件
1: N-bromosuccinmide / tetrachloromethane / 2 h / 10 - 15 °C 2: sodium hydrogencarbonate / ethanol / 2.5 h / 80 °C 3: hydrogenchloride / 1,4-dioxane / 0.5 h / 20 °C View Scheme
参考文献
Packiarajan, Mathivanan; Grenon, Michel; Zorn, Samuel; Hopper, Allen T.; White, Andrew D.; Chandrasena, Gamini; Pu, Xiaosui; Brodbeck, Robbin M.; Robichaud, Albert J.
Bioorganic and Medicinal Chemistry Letters, 2013 , vol. 23, # 14 p. 4037 - 4043
反应条件
1: N-bromosuccinmide / tetrachloromethane / 2 h / 10 - 15 °C 2: sodium hydrogencarbonate / ethanol / 2.5 h / 80 °C 3: hydrogenchloride / 1,4-dioxane / 0.5 h / 20 °C 4: copper(ll) bromide; isopentyl nitrite / acetonitrile / 1.5 h / 20 °C View Scheme
参考文献
Janssen Pharmaceutica N.V.
Patent: US2012/252800 A1, 2012 ;
反应条件
1.1: toluene-4-sulfonic acid / methanol / 1.5 h / Reflux
1.2: 5 h / Reflux
1.3: 20 °C
2.1: lithium hexamethyldisilazane / tetrahydrofuran / 0.5 h
2.2: 3.5 h / 20 °C
3.1: hydrogenchloride; water / tetrahydrofuran / 3 h / 20 °C
View Scheme
参考文献
Almirall, S.A.
Patent: EP2526945 A1, 2012 ;
EP 2526945 A1
反应条件
1: 1-boc-piperidine-2,4-dione With lithium hexamethyldisilazane in tetrahydrofuran
T=-20°C; 0.333333 h;
2: ethyl iodide in tetrahydrofuran
T=-20°C; 2 h;
参考文献
Pharmacia Italia S.p.A.
Patent: US2007/142414 A1, 2007 ;
Location in patent: Page/Page column 18 ;
US 20070142414 A1
反应条件
lithium salt of 1,1,1,3,3,3-hexamethyldisilazane in tetrahydrofuran
T=-20°C; 1.5 h;
参考文献
Orsini, Paolo; Maccario, Alessandro; Colombo, Nicoletta
Synthesis, 2007 , # 20 p. 3185 - 3190