6-氯-4-邻甲苯基-烟酰胺合成路线 (共 5 条)
反应条件
1: With thionyl chloride in tetrahydrofuran; N,N-dimethyl-formamide T=50°C; 2 h; 2: With ammonium hydroxide in tetrahydrofuran; water; N,N-dimethyl-formamide T=0°C; 0.5 h;
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
Location in patent: Page/Page column 25 ;
反应条件
1.1: tetrahydrofuran / 19 h / 0 - 20 °C 1.2: acetic acid / tetrahydrofuran / -60 °C 1.3: Mn(OAc)3*2H2O / tetrahydrofuran / 1.5 h / -60 - 20 °C 2.1: SOCl2; DMF / tetrahydrofuran / 2.5 h / 50 °C 3.1: 7.8 g / NH3 / tetrahydrofuran; H2O / 0.5 h / 0 °C View Scheme
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
反应条件
1.1: tetrahydrofuran / 19 h / 0 - 20 °C 1.2: acetic acid / tetrahydrofuran / -60 °C 1.3: Mn(OAc)3*2H2O / tetrahydrofuran / 1.5 h / -60 - 20 °C 2.1: SOCl2; DMF / tetrahydrofuran / 2.5 h / 50 °C 3.1: 7.8 g / NH3 / tetrahydrofuran; H2O / 0.5 h / 0 °C View Scheme
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
Location in patent: Page/Page column 25 ;
反应条件
1: 2 h / 100 °C 2: 99 percent / N-bromosuccinimide / CH2Cl2; methanol / 7 h / -5 °C 3: Red-Al / toluene; CH2Cl2 / 1 h / 50 °C 4: 13.5 g / i-Pr2NEt / CH2Cl2 / 3 h / 0 °C View Scheme
参考文献
Journal of Organic Chemistry, , vol. 71, # 5 p. 2000 - 2008