N-[[(1,1-二甲基乙基)氨基]羰基]-3-甲基-L-缬氨酸合成路线 (共 6 条)
反应条件
1: (2S)-2-amino-3,3-dimethylbutanoic acid With sodium hydroxide in water pH=11.5; 2: 1,1-dimethylethyl isocyanate in water pH=9.3; Cooling with ice;
参考文献
Kaneka Corporation
Patent: EP2221294 A1, 2010 ;
Location in patent: Page/Page column 6-7 ;
反应条件
1: With 1,1'-carbonyldiimidazole in tetrahydrofuran; dichloromethane T=25 - 30°C; 13.5 h; 2: With hydrogenchloride in tetrahydrofuran; dichloromethane; water pH=2.5; 0.25 h;
参考文献
MSN LABORATORIES LIMITED; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; SAHADEVA REDDY, Maramreddy
Patent: WO2014/61034 A1, 2014 ;
Location in patent: Page/Page column 33; 38 ;
反应条件
1: in dichloromethane T=20 - 30°C; 14 - 16.5 h; Heating / reflux; 2: With hydrogenchloride; water in dichloromethane T=15 - 20°C; pH=1.0 - 2.0; 0.333333 - 1 h; Product distribution / selectivity;
参考文献
WO2009/39361 A2, ;
Page/Page column 7-8 ;
反应条件
1.1: N-ethyl-N,N-diisopropylamine; benzotriazol-1-ol / dichloromethane / 0.17 h / 0 - 5 °C 1.2: 6 h / 25 - 30 °C 2.1: water; lithium hydroxide hydrate / tetrahydrofuran / 6 h / 25 - 30 °C 3.1: N-ethyl-N,N-diisopropylamine; benzotriazol-1-ol; dicyclohexyl-carbodiimide / dichloromethane / 5 h / 0 - 30 °C 4.1: Dess-Martin periodane / dichloromethane / 0 - 30 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; SAHADEVA REDDY, Maramreddy
Patent: WO2014/61034 A1, 2014 ;
反应条件
1: N-ethyl-N,N-diisopropylamine; HATU / acetonitrile / 5 h / 25 - 30 °C 2: Dess-Martin periodane / dichloromethane / 0 - 30 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; SAHADEVA REDDY, Maramreddy
Patent: WO2014/61034 A1, 2014 ;
反应条件
2,6-dimethylpyridine; benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride in acetonitrile
T=10 - 30°C; 3 - 5 h;
参考文献
MSN LABORATORIES LIMITED; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; SAHADEVA REDDY, Maramreddy
Patent: WO2014/61034 A1, 2014 ;
Location in patent: Page/Page column 49-50 ;