1-噁-6-氮杂螺[2.5]辛烷-6-羧酸-1,1-二甲基乙酯合成路线 （共 17 条）
反应条件
ammonia in methanol T=20°C; 72 h;
参考文献
Bioorganic and Medicinal Chemistry Letters, , vol. 20, # 24 p. 7458 - 7461
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 / 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 ;
反应条件
pyridinium poly(hydrogen fluoride) in dichloromethane T=-10 - 20°C;
参考文献
AC Immune S.A.
Patent: EP2377860 A1, 2011 ;
Location in patent: Page/Page column 26 ;
反应条件
1: pyridinium poly(hydrogen fluoride) / dichloromethane / -10 - 20 °C 2: pyridine / 0 - 20 °C 3: N,N-dimethyl-formamide / 12 h / 150 °C 4: ethanolamine / 2.5 h / 60 °C View Scheme
参考文献
AC Immune S.A.
Patent: EP2377860 A1, 2011 ;
反应条件
1.1: isopropylmagnesium chloride / tetrahydrofuran / 0.5 h / 0 °C
1.2: 18 h / 40 °C
2.1: potassium tert-butylate / 40 h / 40 - 50 °C
3.1: hydrogenchloride / tetrahydrofuran
View Scheme
参考文献
Hossain, Nafizal; Ivanova, Svetlana; Bergare, Jonas; Eriksson, Tomas
Bioorganic and Medicinal Chemistry Letters, 2013 , vol. 23, # 6 p. 1883 - 1886
反应条件
1: pyridinium poly(hydrogen fluoride) / dichloromethane / -10 - 20 °C
2: pyridine / 0 - 20 °C
3: N,N-dimethyl-formamide / 12 h / 150 °C
View Scheme
参考文献
AC Immune, S.A.
Patent: US2011/256064 A1, 2011 ;
