4,5-二甲氧基苯并环丁烷-1-甲酸合成路线 （共 7 条）
反应条件
1.1: ethyl acetate / 1.25 h / 0 °C / Reflux 2.1: hydrogenchloride / dichloromethane; water / 0.08 h 3.1: oxalyl dichloride / N,N-dimethyl-formamide / dichloromethane / 15 - 25 °C 4.1: dichloromethane; water / 0 - 10 °C 5.1: borane-THF / tetrahydrofuran / 20 - 50 °C 5.2: 0.25 h / 0 - 5 °C 5.3: 2.5 h / 0 °C / Reflux View Scheme
参考文献
RICHTER GEDEON NYRT.; UJVARI, Viktor; BODI, Jozsef; FARAGO, Janos; SZKE, Katalin; FAIGL, Ferenc; NEMET, Zoltan; TEMESVARI, Krisztina; KISS, Robert; MATRAVOeLGYI, Bela; KASSAI, Ferencne; KISS-BARTOS, Dorottya
Patent: WO2011/138625 A1, 2011 ;
反应条件
1.1: ethyl acetate / 1.25 h / 0 °C / Reflux 2.1: hydrogenchloride / dichloromethane; water / 0.08 h 3.1: oxalyl dichloride / N,N-dimethyl-formamide / dichloromethane / 15 - 25 °C 4.1: dichloromethane; water / 0 - 10 °C 5.1: borane-THF / tetrahydrofuran / 20 - 50 °C 5.2: 0.25 h / 0 - 5 °C 5.3: 2.5 h / 0 °C / Reflux 6.1: potassium carbonate; sodium iodide / 1-methyl-pyrrolidin-2-one / 20 - 60 °C / Inert atmosphere 6.2: 2 h / 20 °C 7.1: potassium carbonate / water / 0.08 h 7.2: Inert atmosphere 8.1: hydrogenchloride; hydrogen / palladium 10 on activated carbon / water / 6 h / 45 °C / 7500.75 Torr View Scheme
参考文献
RICHTER GEDEON NYRT.; UJVARI, Viktor; BODI, Jozsef; FARAGO, Janos; SZKE, Katalin; FAIGL, Ferenc; NEMET, Zoltan; TEMESVARI, Krisztina; KISS, Robert; MATRAVOeLGYI, Bela; KASSAI, Ferencne; KISS-BARTOS, Dorottya
Patent: WO2011/138625 A1, 2011 ;
反应条件
potassium hydroxide in ethanol
5 h; Reflux;
参考文献
Liu, Xin; Liu, Yu; He, Huili; Cai, Zhan; Yang, Yushe
Synthetic Communications, 2014 , vol. 44, # 4 p. 451 - 456
反应条件
1: With potassium hydroxide in water
4 h;
2: With hydrogenchloride in water
0.5 h; Cooling with ice-water bath;
参考文献
RICHTER GEDEON NYRT.; UJVARI, Viktor; BODI, Jozsef; FARAGO, Janos; SZKE, Katalin; FAIGL, Ferenc; NEMET, Zoltan; TEMESVARI, Krisztina; KISS, Robert; MATRAVOeLGYI, Bela; KASSAI, Ferencne; KISS-BARTOS, Dorottya
Patent: WO2011/138625 A1, 2011 ;
Location in patent: Page/Page column 40 ;
反应条件
1: With potassium cyanide in dimethyl sulfoxide
T=130°C; 12 h; Inert atmosphere;
2: With hydrogenchloride; water in diethyl ether; dimethyl sulfoxide
T=20°C; 1 h;
参考文献
LES LABORATOIRES SERVIER; CENTRE NATIONAL DE LA RECHERCHE; UNIVERSITE CLAUDE BERNARD LYON 1
Patent: US2010/16580 A1, 2010 ;
Location in patent: Page/Page column 4 ;
反应条件
1.1: n-butyllithium / hexane; tetrahydrofuran / -10 °C / Inert atmosphere
2.1: potassium hydroxide; water / 4 h / Reflux
2.2: 20 °C
View Scheme
参考文献
RICHTER GEDEON NYRT.; UJVARI, Viktor; BODI, Jozsef; FARAGO, Janos; SZKE, Katalin; FAIGL, Ferenc; NEMET, Zoltan; TEMESVARI, Krisztina; KISS, Robert; MATRAVOeLGYI, Bela; KASSAI, Ferencne; KISS-BARTOS, Dorottya
Patent: WO2011/138625 A1, 2011 ;
反应条件
1.1: ethyl acetate / 1.25 h / 0 °C / Reflux
2.1: hydrogenchloride / dichloromethane; water / 0.08 h
3.1: oxalyl dichloride / N,N-dimethyl-formamide / dichloromethane / 15 - 25 °C
4.1: dichloromethane; water / 0 - 10 °C
5.1: borane-THF / tetrahydrofuran / 20 - 50 °C
5.2: 0.25 h / 0 - 5 °C
5.3: 2.5 h / 0 °C / Reflux
6.1: potassium carbonate; sodium iodide / 1-methyl-pyrrolidin-2-one / 20 - 60 °C / Inert atmosphere
6.2: 2 h / 20 °C
7.1: potassium carbonate / water / 0.08 h
7.2: Inert atmosphere
View Scheme
参考文献
RICHTER GEDEON NYRT.; UJVARI, Viktor; BODI, Jozsef; FARAGO, Janos; SZKE, Katalin; FAIGL, Ferenc; NEMET, Zoltan; TEMESVARI, Krisztina; KISS, Robert; MATRAVOeLGYI, Bela; KASSAI, Ferencne; KISS-BARTOS, Dorottya
Patent: WO2011/138625 A1, 2011 ;
