2-甲基-3-硝基-4-羟基吡啶合成路线 (共 10 条)
反应条件
sulfuric acid; nitric acid T=25 - 130°C;
参考文献
TAKEDA PHARMACEUTICAL COMPANY LIMITED; KWOK, Lily; LARSON, John David; SABAT, Mark
Patent: WO2011/146287 A1, 2011 ;
Location in patent: Page/Page column 59-60 ;
WO 2011/146287 A1
反应条件
1: H2 / PtO2 / acetic acid / 2068.6 Torr 2: 40 percent / HNO3, NaNO2 / H2O / <20 deg C 3: HNO3, H2SO4 / 2 h / Heating View Scheme
参考文献
Reich; Fabio; Lee; Kuck; Testa
Journal of Medicinal Chemistry, 1989 , vol. 32, # 11 p. 2474 - 2485
反应条件
1: 40 percent / HNO3, NaNO2 / H2O / <20 deg C 2: HNO3, H2SO4 / 2 h / Heating View Scheme
参考文献
TAKEDA PHARMACEUTICAL COMPANY LIMITED; KWOK, Lily; LARSON, John David; SABAT, Mark
Patent: WO2011/146287 A1, 2011 ;
WO 2011/146287 A1
反应条件
sulfuric acid; nitric acid 2 h; Heating; Yield given;
参考文献
Reich; Fabio; Lee; Kuck; Testa
Journal of Medicinal Chemistry, 1989 , vol. 32, # 11 p. 2474 - 2485
反应条件
phosphorus oxytribromide T=140°C; 3 h; pressure vessel;
参考文献
TAKEDA PHARMACEUTICAL COMPANY LIMITED; KWOK, Lily; LARSON, John David; SABAT, Mark
Patent: WO2011/146287 A1, 2011 ;
Location in patent: Page/Page column 60 ;
WO 2011/146287 A1
反应条件
in dichloromethane; trichlorophosphate
参考文献
Merck and Co., Inc.
Patent: US5496816 A1, 1996 ;
反应条件
trichlorophosphate 2 h; Heating;
参考文献
Reich; Fabio; Lee; Kuck; Testa
Journal of Medicinal Chemistry, 1989 , vol. 32, # 11 p. 2474 - 2485
反应条件
1.1: phosphorus oxytribromide / 3 h / 140 °C / pressure vessel 2.1: hydrogenchloride; SnCl2·2H2O / water / 1 h / 40 °C 3.1: 4-(N,N-dimethlyamino)pyridine / 60 °C 4.1: sodium hydroxide / methanol / 0.5 h / 20 °C 5.1: acetic anhydride; potassium acetate / toluene / 0.25 h 5.2: 4 h / 85 °C View Scheme
参考文献
WO2011/146287 A1, ;
WO 2011/146287 A1
反应条件
1: 26.7 g / POCl3 / 2 h / Heating 2: N2H4*H2O / ethanol / 1.) 0 deg C, 0.75 h, 2.) 25 deg C, 3.5 h 3: H2 / 5percent Pd/C / aq. ethanol 4: conc. HCl / 2.5 h 5: MnO2, 5 M NaOH / H2O / 0.83 h / pH 6 View Scheme
参考文献
Reich; Fabio; Lee; Kuck; Testa
Journal of Medicinal Chemistry, 1989 , vol. 32, # 11 p. 2474 - 2485
反应条件
1: 26.7 g / POCl3 / 2 h / Heating 2: ethanol / 5 h / Heating 3: H2, HCl / 5percent Pd/C / aq. ethanol / 2327.2 Torr 4: HCl / ethanol / 1.) 25 deg C, 5 h, 2.) reflux, 1.5 h 5: MnO2, 5 M NaOH / H2O / 0.83 h / pH 6 View Scheme
参考文献
Reich; Fabio; Lee; Kuck; Testa
Journal of Medicinal Chemistry, 1989 , vol. 32, # 11 p. 2474 - 2485