6,6-二甲基哌啶-2,4-二酮合成路线 (共 7 条)
反应条件
1: With ethanol; sodium in toluene T=80°C; 2 h; 2: With hydrogenchloride; water in toluene pH=2 - 3; 3: With water in acetonitrile 2 h; Heating / reflux;
参考文献
UCB PHARMA S.A.
Patent: WO2009/71888 A1, 2009 ;
Location in patent: Page/Page column 71-72 ;
WO 2009/071888 A1
反应条件
water in acetonitrile 2 h; Reflux;
参考文献
PHARMACIA and ITALIA S.p.A.
Patent: WO2005/14572 A1, 2005 ;
Location in patent: Page/Page column 28 ;
WO 2005/014572 A1
反应条件
1: in ethanol; toluene T=80°C; 2 h; 2: With water in acetonitrile 2 h; Heating / reflux;
参考文献
UCB PHARMA S.A.
Patent: WO2009/71895 A1, 2009 ;
Location in patent: Page/Page column 94-95 ;
WO 2009/071895 A1
反应条件
hydrogenchloride in water; acetonitrile
参考文献
MAY and BAKER LIMITED
Patent: EP354046 A3, 1990 ;
反应条件
1.1: ammonia / ethanol / 16 h / -70 - 45 °C / 10343.2 Torr / Autoclave 1.2: 0.5 h / 0 °C / pH 2 / Inert atmosphere 2.1: triethylamine / dichloromethane / 3 h / 0 - 20 °C 3.1: sodium ethanolate / toluene / 4 h / 80 °C 4.1: acetonitrile; water / 3 h / Reflux View Scheme
参考文献
AVILA THERAPEUTICS, INC.
Patent: US2011/230476 A1, 2011 ;
反应条件
1: triethylamine / dichloromethane / 3 h / 0 - 20 °C 2: sodium ethanolate / toluene / 4 h / 80 °C 3: acetonitrile; water / 3 h / Reflux View Scheme
参考文献
AVILA THERAPEUTICS, INC.
Patent: US2011/230476 A1, 2011 ;
反应条件
1.1: bromine / tetrahydrofuran / 0.17 h / 20 °C 1.2: 2 h / 80 °C 2.1: copper(ll) bromide; tert.-butylnitrite / acetonitrile / 2 h / 20 °C 3.1: caesium carbonate / palladium diacetate; 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene / acetonitrile / 16 h / 85 °C / Inert atmosphere View Scheme
参考文献
AVILA THERAPEUTICS, INC.
Patent: US2011/230476 A1, 2011 ;