5-氯吡嗪-2-羧酸甲酯合成路线 （共 29 条）
反应条件
1: With trichlorophosphate; N,N-dimethyl-formamide in chloroform 2 h; RefluxInert atmosphere; 2: With sodium hydrogencarbonate in chloroform; water
参考文献
Daiichi Sankyo Company, Limited
Patent: EP2239253 A1, 2010 ;
Location in patent: Page/Page column 96 ;
EP 2239253 A1
反应条件
1: 6-Hydroxy-3-pyridazinecarboxylic acid With thionyl chloride; N,N-dimethyl-formamide in toluene 2 h; Heating / reflux; 2: methanol in toluene T=20°C; 15 h;
参考文献
WO2007/81897 A2, ;
Page/Page column 29 ;
WO 2007/081897 A2
反应条件
1: 6-Hydroxy-3-pyridazinecarboxylic acid With thionyl chloride; N,N-dimethyl-formamide 4 h; Reflux; 2: methanol With pyridine T=20°C;
参考文献
WO2012/40137 A1, ;
Page/Page column 90 ;
WO 2012/040137 A1
反应条件
in methanol; diethyl ether 0.5 h;
参考文献
IRONWOOD PHARMACEUTICALS, INC.; HUDSON, Colleen; BARDEN, Timothy, C.; JIA, James; MERMERIAN, Ara; PENG, Bo; YANG, Jane; YU, Xiang, Y.; SPROTT, Kevin
Patent: WO2012/88469 A1, 2012 ;
Location in patent: Page/Page column 151-152 ;
WO 2012/088469 A1
反应条件
pyridine in dichloromethane 48 h; Ambient temperature;
参考文献
Journal of Medicinal Chemistry, , vol. 38, # 20 p. 3902 - 3907
反应条件
1: 52 percent / POCl3 / 3 h / Heating 2: 76 percent / KMnO4 / tricaprylmethylammonium chloride / benzene; H2O / 4.5 h / 15 - 20 °C 3: 62 percent / HCl (g) / 1 h / Heating View Scheme
参考文献
Journal of Heterocyclic Chemistry, , vol. 19, p. 407 - 408
反应条件
1: 76 percent / KMnO4 / tricaprylmethylammonium chloride / benzene; H2O / 4.5 h / 15 - 20 °C 2: 62 percent / HCl (g) / 1 h / Heating View Scheme
参考文献
Journal of Heterocyclic Chemistry, , vol. 19, p. 407 - 408
反应条件
hydrogenchloride 1 h; Heating; Yields of byproduct given;
参考文献
Sato, Nobuhiro; Arai, Shinji
Journal of Heterocyclic Chemistry, 1982 , vol. 19, p. 407 - 408
反应条件
1: 77 percent / 10percent NaOH / H2O / 3 h / Heating 2: 64 percent / SOCl2 / 2 h / Heating 3: 68 percent / POCl3, DMF / 2 h / Heating View Scheme
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 28, # 10 p. 3057 - 3063
反应条件
1: 26 percent / 10percent Na2CO3 / 8 h / Heating 2: 61 percent / nitrobenzene / 3 h / 170 - 180 °C 3: 77 percent / 10percent NaOH / H2O / 3 h / Heating 4: 64 percent / SOCl2 / 2 h / Heating 5: 68 percent / POCl3, DMF / 2 h / Heating View Scheme
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 28, # 10 p. 3057 - 3063
