N-Boc-4-亚甲基-L-脯氨酸合成路线 （共 18 条）
反应条件
1.1: potassium carbonate; N,N-dimethyl-formamide / 7 h / 20 °C 2.1: tetrabutylammomium bromide / 1,2-dichloro-ethane / 3.17 h / 70 °C / Inert atmosphere 3.1: 2,2'-azo-bisisobutyronitrile; tris-(trimethylsilyl)silane / toluene / 24 h / 0 - 90 °C 4.1: water; lithium hydroxide hydrate / ethanol / 20 h / 20 °C 4.2: pH 2 / Ice bath View Scheme
反应条件
diethylzinc in n-heptane; dichloromethane
T=-5 - 20°C; 19.5 h; Overall yield = 62 percent; Overall yield = 46.6 g;
参考文献
Gilead Sciences, Inc.; Scott, Robert William; Vitale, Justin Philip; Matthews, Kenneth Stanley; Teresk, Martin Gerald; Formella, Alexandra; Evans, Jared Wayne
Patent: US2013/324740 A1, 2013 ;
Location in patent: Paragraph 0131; 0132; 0133 ;
反应条件
1: potassium carbonate; N,N-dimethyl-formamide / 7 h / 20 °C
2: tetrabutylammomium bromide / 1,2-dichloro-ethane / 3.17 h / 70 °C / Inert atmosphere
3: 2,2'-azo-bisisobutyronitrile; tris-(trimethylsilyl)silane / toluene / 24 h / 0 - 90 °C
View Scheme
参考文献
GLAXOSMITHKLINE LLC; BASKARAN, Subramanian; BOTYANSZKI, Janos; COOPER, Joel P.; DUAN, Maosheng; KAZMIERSKI, Wieslaw Mieczyslaw; MCFADYEN, Robert Blount; REDMAN, Aniko
Patent: WO2011/50146 A1, 2011 ;
反应条件
potassium carbonate; N,N-dimethyl-formamide
T=20°C; 7 h;
参考文献
ENANTA PHARMACEUTICALS, INC.; QIU, Yao-Ling; PENG, Xiaowen; KIM, In, Jong; CAO, Hui; TANG, Datong; OR, Yat, Sun; WANG, Guoqiang; XU, Guoyou
Patent: WO2012/158861 A2, 2012 ;
Location in patent: Page/Page column 20 ;
反应条件
diethylzinc in n-heptane; dichloromethane
T=-5 - 20°C; 19.5 h; Overall yield = 62 percent; Overall yield = 46.6 g;
参考文献
Gilead Sciences, Inc.; Scott, Robert William; Vitale, Justin Philip; Matthews, Kenneth Stanley; Teresk, Martin Gerald; Formella, Alexandra; Evans, Jared Wayne
Patent: US2013/324740 A1, 2013 ;
Location in patent: Paragraph 0131; 0132; 0133 ;
反应条件
in methanol; hexane; dichloromethane
参考文献
GLAXOSMITHKLINE LLC; BASKARAN, Subramanian; BOTYANSZKI, Janos; COOPER, Joel P.; DUAN, Maosheng; KAZMIERSKI, Wieslaw Mieczyslaw; MCFADYEN, Robert Blount; REDMAN, Aniko
Patent: WO2011/50146 A1, 2011 ;
Location in patent: Page/Page column 42 ;
反应条件
in chloroform
Yield given;
参考文献
Herdewijn; Claes; Vanderhaeghe
Canadian Journal of Chemistry, 1982 , vol. 60, # 23 p. 2903 - 2907
反应条件
1: CHCl3
2: 85 percent / 98percent HCOOH / 2.5 h / Ambient temperature
View Scheme
参考文献
Herdewijn; Claes; Vanderhaeghe
Canadian Journal of Chemistry, 1982 , vol. 60, # 23 p. 2903 - 2907
