甲氧基-9-椭圆玫瑰树碱乳酸盐合成路线 (共 24 条)
反应条件
1: 9-methoxy-5,11-dimethyl-6H-pyrido[4,3-b]carbazole With sodium hydride in N,N-dimethyl-formamide T=0°C; 0.5 h; 2: methyl iodide in N,N-dimethyl-formamide T=0 - 20°C;
参考文献
Vehar, Blaz; Hrast, Martina; Kovac, Andreja; Konc, Janez; Mariner, Katherine; Chopra, Ian; O'Neill, Alex; Janezic, Dusanka; Gobec, Stanislav
Bioorganic and Medicinal Chemistry, 2011 , vol. 19, # 17 p. 5137 - 5146
反应条件
in N-methyl-acetamide
参考文献
Hoffmann-La Roche Inc.
Patent: US3933827 A1, 1976 ;
反应条件
1: 53 percent / Copper bronze, K2CO3 / I2 / 24 h / 120 °C
2: Hydrazine hydrate (98percent) / Raney Ni / aq. ethanol / 1 h / Heating
3: 94 percent / 1.) aqueous NaNO2 / acetic acid; H2O / 1.) 0 deg C, 2.) 2 h, 0 deg C bis room temp.
4: 62 percent / acetone; methanol / 500 °C
View Scheme
参考文献
Miller; Stowell
Journal of Organic Chemistry, 1983 , vol. 48, # 6 p. 886 - 888
反应条件
1: 53 percent / Copper bronze, K2CO3 / I2 / 24 h / 120 °C
2: Hydrazine hydrate (98percent) / Raney Ni / aq. ethanol / 1 h / Heating
3: 94 percent / 1.) aqueous NaNO2 / acetic acid; H2O / 1.) 0 deg C, 2.) 2 h, 0 deg C bis room temp.
4: 62 percent / acetone; methanol / 500 °C
View Scheme
参考文献
Miller; Stowell
Journal of Organic Chemistry, 1983 , vol. 48, # 6 p. 886 - 888
反应条件
in 1,3,5-trimethyl-benzene
5 h; Heating;
参考文献
Liu, Ching-Yuan; Knochel, Paul
Journal of Organic Chemistry, 2007 , vol. 72, # 19 p. 7106 - 7115
反应条件
1.1: potassium hydroxide / H2O / 5 h / Heating
1.2: 83 percent / sulfuric acid / H2O / 20 h / Heating
2.1: 88 percent / polyphosphoric acid / 2.5 h / 100 °C
3.1: 98 percent / sodium borohydride / ethanol / 1 h / 0 - 20 °C
4.1: 86 percent / p-toluenesulfonic acid / benzene / 2 h / Heating
5.1: ozone / methanol; CH2Cl2 / -78 °C
5.2: dimethyl sulfide; sodium hydrogen carbonate / methanol; CH2Cl2 / 4 h / 20 °C
6.1: 101 mg / aq. NH3 / CH2Cl2; methanol / 12 h / 20 °C
7.1: i-PrMgCl*LiCl / tetrahydrofuran / 1.2 h / -20 - -10 °C
7.2: ZnBr2 / tetrahydrofuran / 0.5 h / -10 - -5 °C
7.3: 63 percent / Pd(PPh3)4 / tetrahydrofuran / 5 h / Heating
8.1: 94 percent / potassium hydrogen sulfate; sodium azide / CH2Cl2; H2O / 12 h / 20 °C
9.1: 68 percent / 1,3,5-trimethyl-benzene / 5 h / Heating
View Scheme
参考文献
Liu, Ching-Yuan; Knochel, Paul
Journal of Organic Chemistry, 2007 , vol. 72, # 19 p. 7106 - 7115
反应条件
1.1: 88 percent / polyphosphoric acid / 2.5 h / 100 °C
2.1: 98 percent / sodium borohydride / ethanol / 1 h / 0 - 20 °C
3.1: 86 percent / p-toluenesulfonic acid / benzene / 2 h / Heating
4.1: ozone / methanol; CH2Cl2 / -78 °C
4.2: dimethyl sulfide; sodium hydrogen carbonate / methanol; CH2Cl2 / 4 h / 20 °C
5.1: 101 mg / aq. NH3 / CH2Cl2; methanol / 12 h / 20 °C
6.1: i-PrMgCl*LiCl / tetrahydrofuran / 1.2 h / -20 - -10 °C
6.2: ZnBr2 / tetrahydrofuran / 0.5 h / -10 - -5 °C
6.3: 63 percent / Pd(PPh3)4 / tetrahydrofuran / 5 h / Heating
7.1: 94 percent / potassium hydrogen sulfate; sodium azide / CH2Cl2; H2O / 12 h / 20 °C
8.1: 68 percent / 1,3,5-trimethyl-benzene / 5 h / Heating
View Scheme
参考文献
Liu, Ching-Yuan; Knochel, Paul
Journal of Organic Chemistry, 2007 , vol. 72, # 19 p. 7106 - 7115
反应条件
1.1: 98 percent / sodium borohydride / ethanol / 1 h / 0 - 20 °C
2.1: 86 percent / p-toluenesulfonic acid / benzene / 2 h / Heating
3.1: ozone / methanol; CH2Cl2 / -78 °C
3.2: dimethyl sulfide; sodium hydrogen carbonate / methanol; CH2Cl2 / 4 h / 20 °C
4.1: 101 mg / aq. NH3 / CH2Cl2; methanol / 12 h / 20 °C
5.1: i-PrMgCl*LiCl / tetrahydrofuran / 1.2 h / -20 - -10 °C
5.2: ZnBr2 / tetrahydrofuran / 0.5 h / -10 - -5 °C
5.3: 63 percent / Pd(PPh3)4 / tetrahydrofuran / 5 h / Heating
6.1: 94 percent / potassium hydrogen sulfate; sodium azide / CH2Cl2; H2O / 12 h / 20 °C
7.1: 68 percent / 1,3,5-trimethyl-benzene / 5 h / Heating
View Scheme
参考文献
Liu, Ching-Yuan; Knochel, Paul
Journal of Organic Chemistry, 2007 , vol. 72, # 19 p. 7106 - 7115
反应条件
1.1: 86 percent / p-toluenesulfonic acid / benzene / 2 h / Heating
2.1: ozone / methanol; CH2Cl2 / -78 °C
2.2: dimethyl sulfide; sodium hydrogen carbonate / methanol; CH2Cl2 / 4 h / 20 °C
3.1: 101 mg / aq. NH3 / CH2Cl2; methanol / 12 h / 20 °C
4.1: i-PrMgCl*LiCl / tetrahydrofuran / 1.2 h / -20 - -10 °C
4.2: ZnBr2 / tetrahydrofuran / 0.5 h / -10 - -5 °C
4.3: 63 percent / Pd(PPh3)4 / tetrahydrofuran / 5 h / Heating
5.1: 94 percent / potassium hydrogen sulfate; sodium azide / CH2Cl2; H2O / 12 h / 20 °C
6.1: 68 percent / 1,3,5-trimethyl-benzene / 5 h / Heating
View Scheme
参考文献
Liu, Ching-Yuan; Knochel, Paul
Journal of Organic Chemistry, 2007 , vol. 72, # 19 p. 7106 - 7115
反应条件
1.1: ozone / methanol; CH2Cl2 / -78 °C
1.2: dimethyl sulfide; sodium hydrogen carbonate / methanol; CH2Cl2 / 4 h / 20 °C
2.1: 101 mg / aq. NH3 / CH2Cl2; methanol / 12 h / 20 °C
3.1: i-PrMgCl*LiCl / tetrahydrofuran / 1.2 h / -20 - -10 °C
3.2: ZnBr2 / tetrahydrofuran / 0.5 h / -10 - -5 °C
3.3: 63 percent / Pd(PPh3)4 / tetrahydrofuran / 5 h / Heating
4.1: 94 percent / potassium hydrogen sulfate; sodium azide / CH2Cl2; H2O / 12 h / 20 °C
5.1: 68 percent / 1,3,5-trimethyl-benzene / 5 h / Heating
View Scheme
参考文献
Liu, Ching-Yuan; Knochel, Paul
Journal of Organic Chemistry, 2007 , vol. 72, # 19 p. 7106 - 7115