2,6-二氯-5-氟烟酰乙酸乙酯合成路线 （共 28 条）
反应条件
toluene-4-sulfonic acid in water 2 h; Heating; Yield given;
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 38, # 12 p. 3211 - 3217
反应条件
1: With zinc(II) chloride in 1,2-dichloro-ethane Heating / reflux; 2: With hydrogenchloride; water in 1,2-dichloro-ethane T=90°C; 4 h; Product distribution / selectivity;
参考文献
LG LIFE SCIENCES LTD.
Patent: WO2007/64077 A1, 2007 ;
Location in patent: Page/Page column 7 ;
反应条件
n-butyllithium; biquinoline 1.) THF, hexane, from -30 deg C to -5 deg C, 2.) THF, hexane, RT, 1 h; Yield given. Multistep reaction;
参考文献
Journal of Medicinal Chemistry, , vol. 29, # 11 p. 2364 - 2369
反应条件
1: 5-fluoro-2,6-dihydroxynicotinonitrile With phosphorus pentachloride; trichlorophosphate Heating / reflux; 2: malonic acid ethyl ester monopotassium salt With zinc(II) chloride in 1,2-dichloro-ethane Heating / reflux; 3: With hydrogenchloride; water in 1,2-dichloro-ethane T=90°C; 4 h; Product distribution / selectivity;
参考文献
LG LIFE SCIENCES LTD.
Patent: WO2007/64077 A1, 2007 ;
Location in patent: Page/Page column 6 ;
反应条件
1: SOCl2, DMF / toluene / 3 h / Heating 2: 99 percent / MgCl2, 2-methylimidazole / tetrahydrofuran / 1.) 22 deg C, 20 min; 10 deg C, 20 min, 2.) r.t., 18 h 3: 70 percent / pyridinium tosylate / ethanol / 18 h / Heating View Scheme
参考文献
Organic Preparations and Procedures International, , vol. 29, # 2 p. 231 - 234
反应条件
potassium tert-butylate in 1,4-dioxane 2 h; Ambient temperature;
参考文献
Miyamoto; Matsumoto
Chemical and Pharmaceutical Bulletin, 1990 , vol. 38, # 12 p. 3211 - 3217
反应条件
1: 35 percent / tri-n-butylphosphine / diisopropyl ether / 18 h / Ambient temperature 2: 37 percent / KOtBu / dioxane / 2 h / Ambient temperature View Scheme
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 38, # 12 p. 3211 - 3217
反应条件
1: 99 percent / MgCl2, 2-methylimidazole / tetrahydrofuran / 1.) 22 deg C, 20 min; 10 deg C, 20 min, 2.) r.t., 18 h 2: 70 percent / pyridinium tosylate / ethanol / 18 h / Heating View Scheme
参考文献
Organic Preparations and Procedures International, , vol. 29, # 2 p. 231 - 234
反应条件
1: 73.2 percent / trifluoroacetic acid, 7.5 N aq. HCl / 24 h / Heating 2: thionyl chloride / 2 h / 80 °C 3: 1.) n-BuLi, biquinoline / 1.) THF, hexane, from -30 deg C to -5 deg C, 2.) THF, hexane, RT, 1 h View Scheme
参考文献
Journal of Medicinal Chemistry, , vol. 29, # 11 p. 2364 - 2369
反应条件
1: 1.) conc. H2SO4 / 1.) 65-75 deg C, 1 h, 2.) H2O, 100-110 deg C, 1.5 h 2: 81 percent / SOCl2 / 1 h / Heating 3: 1.) Mg, CCl4, EtOH / 1.) Et2O, reflux, 30 min, 2.) 10 min 4: p-toluenesulfonic acid / H2O / 2 h / Heating View Scheme
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 38, # 12 p. 3211 - 3217
