4-(羟基甲基)-4-甲氧基哌啶-1-羧酸叔丁酯合成路线 (共 7 条)
反应条件
20 palladium(II) hydroxide on carbon; hydrogen in methanol T=20°C; 4 h; Inert atmosphere;
参考文献
Astellas Pharma Inc.; SAMIZU, Kiyohiro; MASUDA, Naoyuki; IIKUBO, Kazuhiko; KOGANEMARU, Yohei; KAWANO, Noriyuki; OHMORI, Junya; MITANI, Yasuyuki; NI, Keni
Patent: EP2565194 A1, 2013 ;
Location in patent: Paragraph 0072 ;
反应条件
in methanol; ethyl acetate
参考文献
Takeda Chemical Industries, Ltd.
Patent: US6403595 B1, 2002 ;
US 6403595 B1
反应条件
1.1: sodium hydride; tetra-(n-butyl)ammonium iodide / tetrahydrofuran; mineral oil / 3 h / 20 °C / |Cooling with ice 2.1: 3-chloro-benzenecarboperoxoic acid / chloroform / 1 h / 20 °C 3.1: lithium aluminium tetrahydride / diethyl ether / 1 h / 20 °C / |Cooling with ice 3.2: 2 h / 20 °C / |Cooling with ice 4.1: sodium hydride / mineral oil; N,N-dimethyl-formamide / 0.67 h / 50 °C / |Cooling with ice 4.2: 4 h / 20 °C 5.1: 20 palladium(II) hydroxide on carbon; hydrogen / methanol / 4 h / 20 °C / |Inert atmosphere View Scheme
参考文献
Astellas Pharma Inc.; SAMIZU, Kiyohiro; MASUDA, Naoyuki; IIKUBO, Kazuhiko; KOGANEMARU, Yohei; KAWANO, Noriyuki; OHMORI, Junya; MITANI, Yasuyuki; NI, Keni
Patent: EP2565194 A1, 2013 ;
反应条件
1.1: 3-chloro-benzenecarboperoxoic acid / chloroform / 1 h / 20 °C 2.1: lithium aluminium tetrahydride / diethyl ether / 1 h / 20 °C / |Cooling with ice 2.2: 2 h / 20 °C / |Cooling with ice 3.1: sodium hydride / mineral oil; N,N-dimethyl-formamide / 0.67 h / 50 °C / |Cooling with ice 3.2: 4 h / 20 °C 4.1: 20 palladium(II) hydroxide on carbon; hydrogen / methanol / 4 h / 20 °C / |Inert atmosphere View Scheme
参考文献
Astellas Pharma Inc.; SAMIZU, Kiyohiro; MASUDA, Naoyuki; IIKUBO, Kazuhiko; KOGANEMARU, Yohei; KAWANO, Noriyuki; OHMORI, Junya; MITANI, Yasuyuki; NI, Keni
Patent: EP2565194 A1, 2013 ;
反应条件
1.1: lithium aluminium tetrahydride / diethyl ether / 1 h / 20 °C / |Cooling with ice 1.2: 2 h / 20 °C / |Cooling with ice 2.1: sodium hydride / mineral oil; N,N-dimethyl-formamide / 0.67 h / 50 °C / |Cooling with ice 2.2: 4 h / 20 °C 3.1: 20 palladium(II) hydroxide on carbon; hydrogen / methanol / 4 h / 20 °C / |Inert atmosphere View Scheme
参考文献
Astellas Pharma Inc.; SAMIZU, Kiyohiro; MASUDA, Naoyuki; IIKUBO, Kazuhiko; KOGANEMARU, Yohei; KAWANO, Noriyuki; OHMORI, Junya; MITANI, Yasuyuki; NI, Keni
Patent: EP2565194 A1, 2013 ;
反应条件
1.1: sodium hydride / mineral oil; N,N-dimethyl-formamide / 0.67 h / 50 °C / |Cooling with ice 1.2: 4 h / 20 °C 2.1: 20 palladium(II) hydroxide on carbon; hydrogen / methanol / 4 h / 20 °C / |Inert atmosphere View Scheme
参考文献
Astellas Pharma Inc.; SAMIZU, Kiyohiro; MASUDA, Naoyuki; IIKUBO, Kazuhiko; KOGANEMARU, Yohei; KAWANO, Noriyuki; OHMORI, Junya; MITANI, Yasuyuki; NI, Keni
Patent: EP2565194 A1, 2013 ;
反应条件
1.1: sodium hydride / mineral oil; N,N-dimethyl-formamide / 0.67 h / 20 °C / |Cooling with ice 1.2: 4 h / 20 °C 2.1: sodium hydride / mineral oil; N,N-dimethyl-formamide / 0.67 h / 50 °C / |Cooling with ice 2.2: 4 h / 20 °C 3.1: 20 palladium(II) hydroxide on carbon; hydrogen / methanol / 4 h / 20 °C / |Inert atmosphere View Scheme
参考文献
Astellas Pharma Inc.; SAMIZU, Kiyohiro; MASUDA, Naoyuki; IIKUBO, Kazuhiko; KOGANEMARU, Yohei; KAWANO, Noriyuki; OHMORI, Junya; MITANI, Yasuyuki; NI, Keni
Patent: EP2565194 A1, 2013 ;