2-(1-苄基-1H-吲哚-5-基)乙烷磺酸甲酰胺合成路线 （共 11 条）
反应条件
1: 75 percent / trifluoroacetic acid; acetic acid / 1 h / 100 °C 2: 74 percent / H2 / 10 percent Pd/C / tetrahydrofuran / 4 h / 20 °C / 3750.3 Torr 3: 84 percent / Na; liquid NH3 / tetrahydrofuran / 0.17 h View Scheme
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
反应条件
1.1: potassium hydroxide / methanol / 8 h / 60 - 65 °C 2.1: trifluoroacetic acid / dichloromethane / 0.17 h / 25 °C 2.2: 25 - 30 °C 2.3: 10 - 15 °C 3.1: hydrogen; acetic acid / palladium 10 on activated carbon / 25 °C / 724.03 Torr 3.2: 10 °C / pH 7.5 - 8.5 4.1: hydrogenchloride / isopropyl alcohol; acetone / 5 - 10 °C / pH 1 View Scheme
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
反应条件
hydrogen; palladium on activated charcoal in methanol
T=20°C; P=3750.3 Torr; 2 h;
参考文献
Poszavacz, Laszlo; Simig, Gyula; Fetter, Jozsef; Bertha, Ferenc
Heterocycles, 2006 , vol. 68, # 4 p. 713 - 719
反应条件
potassium tert-butylate in 1-methyl-pyrrolidin-2-one
T=80 - 85°C;
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
Location in patent: Page/Page column 36 ;
反应条件
1.1: 75 percent / DDQ / CH2Cl2 / 3 h / 0 °C
2.1: t-BuOK / tetrahydrofuran / 1 h / -78 °C
2.2: 73 percent / tetrahydrofuran / -78 - 0 °C
3.1: 84 percent / H2 / 10 percent Pd/C / methanol / 2 h / 20 °C / 3750.3 Torr
View Scheme
参考文献
Poszavacz, Laszlo; Simig, Gyula; Fetter, Jozsef; Bertha, Ferenc
Heterocycles, 2006 , vol. 68, # 4 p. 713 - 719
反应条件
1.1: t-BuOK / tetrahydrofuran / 1 h / -78 °C
1.2: 73 percent / tetrahydrofuran / -78 - 0 °C
2.1: 84 percent / H2 / 10 percent Pd/C / methanol / 2 h / 20 °C / 3750.3 Torr
View Scheme
参考文献
Poszavacz, Laszlo; Simig, Gyula; Fetter, Jozsef; Bertha, Ferenc
Heterocycles, 2006 , vol. 68, # 4 p. 713 - 719
反应条件
1.1: sodium hydrogencarbonate; iodine / dichloromethane / 25 - 30 °C
2.1: methanol / 25 - 30 °C
2.2: 4 h / 25 - 30 °C
3.1: copper(l) iodide; lithium chloride / N,N-dimethyl-formamide / 0.5 h / 25 °C
3.2: 25 °C
4.1: potassium hydroxide; ethanol / 15 - 25 °C
5.1: potassium tert-butylate / 1-methyl-pyrrolidin-2-one / 80 - 85 °C
View Scheme
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
反应条件
1.1: copper(l) iodide; lithium chloride / N,N-dimethyl-formamide / 0.5 h / 25 °C
1.2: 25 °C
2.1: potassium hydroxide; ethanol / 15 - 25 °C
3.1: potassium tert-butylate / 1-methyl-pyrrolidin-2-one / 80 - 85 °C
View Scheme
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
反应条件
1: potassium hydroxide; ethanol / 15 - 25 °C
2: potassium tert-butylate / 1-methyl-pyrrolidin-2-one / 80 - 85 °C
View Scheme
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
反应条件
1.1: methanol / 25 - 30 °C
1.2: 4 h / 25 - 30 °C
2.1: copper(l) iodide; lithium chloride / N,N-dimethyl-formamide / 0.5 h / 25 °C
2.2: 25 °C
3.1: potassium hydroxide; ethanol / 15 - 25 °C
4.1: potassium tert-butylate / 1-methyl-pyrrolidin-2-one / 80 - 85 °C
View Scheme
参考文献
CIPLA LIMITED; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; CHIKHALIKAR, Sandip Vasant; GHAGARE, Maruti; CURTIS, Philip Anthony
Patent: WO2011/21000 A2, 2011 ;
