7-氯-2-氧代-1,2-二氢螺[哌啶-4,4-吡啶并[2,3-d][1,3]噁嗪]-1-羧酸苄酯合成路线 （共 4 条）
反应条件
hydrogen; palladium 10 on activated carbon in ethanol P=760.051 Torr; 24 h;
参考文献
MERCK and CO., INC.
Patent: WO2006/41830 A2, 2006 ;
Location in patent: Page/Page column 55 ;
WO 2006/041830 A2
反应条件
1: 1,1-dimethylethyl[6-chloro-2-pyridinyl]carbamate With n-butyllithium; N,N,N',N,-tetramethylethylenediamine in tetrahydrofuran
T=-78°C; 2.83333 h; Inert atmosphere;
2: 1-benzyloxycarbonyl-piperidin-4-one in tetrahydrofuran
T=-78 - 40°C; Inert atmosphere;
3: With water; sodium hydrogencarbonate in tetrahydrofuran
参考文献
BOEHRINGER INGELHEIM INTERNATIONAL GMBH
Patent: US2012/149698 A1, 2012 ;
Location in patent: Page/Page column 26 ;
反应条件
1: With n-butyllithium; N,N,N',N,-tetramethylethylenediamine in tetrahydrofuran
T=-78 - -20°C; 0.666667 h;
2: 1,1-dimethylethyl[6-chloro-2-pyridinyl]carbamate in tetrahydrofuran
T=-78 - -50°C; 3.25 h;
3: 1-benzyloxycarbonyl-piperidin-4-one in tetrahydrofuran
T=-50 - 20°C; 24 h;
参考文献
MERCK and CO., INC.
Patent: WO2007/16087 A2, 2007 ;
Location in patent: Page/Page column 49; 66 ;
WO 2007/016087 A2
反应条件
1.1: sodium hexamethyldisilazane / tetrahydrofuran / 20 °C / Inert atmosphere
2.1: N,N,N',N,-tetramethylethylenediamine; n-butyllithium / tetrahydrofuran / 2.5 h / -78 °C / Inert atmosphere
2.2: 19 h / -78 - 40 °C
View Scheme
参考文献
Boehringer Ingelheim International GmbH
Patent: US2011/172218 A1, 2011 ;
US 20110172218 A1
