2,5-二氨基-苯磺酰胺合成路线 (共 13 条)
反应条件
hydrogen; palladium 10 on activated carbon in tetrahydrofuran; methanol T=23°C; P=2585.81 Torr; autoclaveInert atmosphereIndustry scale;
参考文献
ANADYS PHARMACEUTICALS, INC.
Patent: WO2008/124450 A1, 2008 ;
Location in patent: Page/Page column 70 ;
反应条件
hydrogen; palladium on activated carbon in methanol; water T=55°C; 16 h; Product distribution / selectivity;
参考文献
ANADYS PHARMACEUTICALS, INC.
Patent: WO2008/73982 A2, 2008 ;
Location in patent: Page/Page column 72 ;
反应条件
sulfuric acid in water T=130°C; 2.5 h; Product distribution / selectivity;
参考文献
ANADYS PHARMACEUTICALS, INC.
Patent: WO2008/73982 A2, 2008 ;
Location in patent: Page/Page column 67 ;
反应条件
1: 90 percent / (NH4)2CO3; CuSO4; aq. NH3 / 4 h / 120 °C 2: 70 percent / Na2S2O4; aq. NaOH View Scheme
参考文献
Ismail, Mohamed A.H.; Abou El Ella, Dalal A.; Abouzid, Khaled A.M.; Mahmoud, Amr H.
Bioorganic and Medicinal Chemistry, 2013 , vol. 21, # 17 p. 5647 - 5647
反应条件
1.1: trichlorophosphate / sulfolane / 80 - 120 °C 1.2: 10 - 95 °C 1.3: 25 - 80 °C / pH 6 - 8 2.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran; methanol / 23 °C / 2585.81 Torr / Industry scale; Autoclave View Scheme
参考文献
ANADYS PHARMACEUTICALS, INC.
Patent: WO2008/124450 A1, 2008 ;
反应条件
1.1: ammonium hydroxide / toluene; water; tetrahydrofuran / 2 h / -10 °C / Reflux 1.2: pH 4 2.1: ammonium hydroxide; (NH4)2CO3; copper(II) sulfate / water / 72 h / 118 °C / Autoclave; Industry scale 3.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran; methanol / 23 °C / 2585.81 Torr / Industry scale; Autoclave View Scheme
参考文献
ANADYS PHARMACEUTICALS, INC.
Patent: WO2008/124450 A1, 2008 ;
反应条件
1.1: N,N-dimethyl-formamide; thionyl chloride / 4 h / Reflux 2.1: ammonium hydroxide / toluene; water; tetrahydrofuran / 2 h / -10 °C / Reflux 2.2: pH 4 3.1: ammonium hydroxide; (NH4)2CO3; copper(II) sulfate / water / 72 h / 118 °C / Autoclave; Industry scale 4.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran; methanol / 23 °C / 2585.81 Torr / Industry scale; Autoclave View Scheme
参考文献
ANADYS PHARMACEUTICALS, INC.
Patent: WO2008/124450 A1, 2008 ;
反应条件
1: sulfuric acid; nitric acid / 21 h / 0 - 20 °C 2: sulfuric acid / 130 °C 3: palladium 10 on activated carbon; hydrogen / tetrahydrofuran / 5 h / 25 °C / 760.05 Torr View Scheme
参考文献
Ismail, Mohamed A.H.; Abou El Ella, Dalal A.; Abouzid, Khaled A.M.; Mahmoud, Amr H.
Bioorganic and Medicinal Chemistry, 2013 , vol. 21, # 17 p. 5647 - 5647
反应条件
1: palladium 10 on activated carbon; hydrazine hydrate / ethanol / 1.5 h / Reflux 2: 0.5 h / 180 °C 3: sulfuric acid; nitric acid / 21 h / 0 - 20 °C 4: sulfuric acid / 130 °C 5: palladium 10 on activated carbon; hydrogen / tetrahydrofuran / 5 h / 25 °C / 760.05 Torr View Scheme
参考文献
Ismail, Mohamed A.H.; Abou El Ella, Dalal A.; Abouzid, Khaled A.M.; Mahmoud, Amr H.
Bioorganic and Medicinal Chemistry, 2013 , vol. 21, # 17 p. 5647 - 5647
反应条件
1: 0.5 h / 180 °C 2: sulfuric acid; nitric acid / 21 h / 0 - 20 °C 3: sulfuric acid / 130 °C 4: palladium 10 on activated carbon; hydrogen / tetrahydrofuran / 5 h / 25 °C / 760.05 Torr View Scheme
参考文献
Ismail, Mohamed A.H.; Abou El Ella, Dalal A.; Abouzid, Khaled A.M.; Mahmoud, Amr H.
Bioorganic and Medicinal Chemistry, 2013 , vol. 21, # 17 p. 5647 - 5647