2-氰基-4-氟-6-甲基-苯甲酸甲酯合成路线 (共 9 条)
反应条件
palladium diacetate; sodium carbonate in 1-methyl-pyrrolidin-2-one
T=120°C; Inert atmosphereSealed tube;
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
Location in patent: Page/Page column 27; 29 ;
反应条件
in N,N-dimethyl-formamide
T=110°C; 5 h;
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
Location in patent: Page/Page column 30; 31 ;
反应条件
1.1: sulfuric acid / water / 150 °C
2.1: sodium nitrite; sulfuric acid / water / 1 h / 80 °C
2.2: 20 °C
3.1: potassium carbonate / N,N-dimethyl-formamide / 23 h / 20 °C
4.1: sodium carbonate; palladium diacetate / 1-methyl-pyrrolidin-2-one / 120 °C / |Inert atmosphere; |Sealed tube
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
反应条件
1.1: sodium nitrite; sulfuric acid / water / 1 h / 80 °C
1.2: 20 °C
2.1: potassium carbonate / N,N-dimethyl-formamide / 23 h / 20 °C
3.1: sodium carbonate; palladium diacetate / 1-methyl-pyrrolidin-2-one / 120 °C / |Inert atmosphere; |Sealed tube
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
反应条件
1: potassium carbonate / N,N-dimethyl-formamide / 23 h / 20 °C
2: sodium carbonate; palladium diacetate / 1-methyl-pyrrolidin-2-one / 120 °C / |Inert atmosphere; |Sealed tube
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
反应条件
1.1: palladium diacetate; [bis(acetoxy)iodo]benzene; iodine / N,N-dimethyl-formamide / 18 h / 100 °C / |Inert atmosphere
2.1: potassium carbonate / N,N-dimethyl-formamide / 0.25 h
2.2: 2 h / 20 °C
3.1: N,N-dimethyl-formamide / 5 h / 110 °C
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
反应条件
1.1: potassium carbonate / N,N-dimethyl-formamide / 0.25 h
1.2: 2 h / 20 °C
2.1: N,N-dimethyl-formamide / 5 h / 110 °C
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
反应条件
1.1: N-bromosuccinmide / N,N-dimethyl-formamide / 20 °C
2.1: hydrogenchloride / water / 2 °C
2.2: 5 °C / pH Ca. 7
2.3: 5 - 70 °C
3.1: sulfuric acid / water / 150 °C
4.1: sodium nitrite; sulfuric acid / water / 1 h / 80 °C
4.2: 20 °C
5.1: potassium carbonate / N,N-dimethyl-formamide / 23 h / 20 °C
6.1: sodium carbonate; palladium diacetate / 1-methyl-pyrrolidin-2-one / 120 °C / |Inert atmosphere; |Sealed tube
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;
反应条件
1.1: hydrogenchloride / water / 2 °C
1.2: 5 °C / pH Ca. 7
1.3: 5 - 70 °C
2.1: sulfuric acid / water / 150 °C
3.1: sodium nitrite; sulfuric acid / water / 1 h / 80 °C
3.2: 20 °C
4.1: potassium carbonate / N,N-dimethyl-formamide / 23 h / 20 °C
5.1: sodium carbonate; palladium diacetate / 1-methyl-pyrrolidin-2-one / 120 °C / |Inert atmosphere; |Sealed tube
View Scheme
参考文献
NERVIANO MEDICAL SCIENCES S.R.L.; PAPEO, Gianluca Mariano Enrico; KRASAVIN, Mikhail Yurievitch; ORSINI, Paolo; SCOLARO, Alessandra
Patent: WO2014/64149 A1, 2014 ;