2-碘-5-甲基苯甲酸甲酯合成路线 （共 13 条）
反应条件
sulfuric acid T=17 - 64.6°C; 18 h;
参考文献
MERCK and CO., INC.; MERCK FROSST CANADA LTD.
Patent: WO2009/143033 A1, 2009 ;
Location in patent: Page/Page column 28-29 ;
WO 2009/143033 A1
反应条件
copper(l) iodide; diiodomethane; isopentyl nitrite in tetrahydrofuran T=70°C; 1.5 h;
参考文献
Dainippon Sumitomo Pharma Co., Ltd.; AstraZeneca AB
Patent: EP1939202 A1, 2008 ;
Location in patent: Page/Page column 54-55 ;
反应条件
sulfuric acid in methanol T=65°C; Fischer–Speier Esterification; 18 h; Large scale;
参考文献
Girardin, Melina; Ouellet, Stephane G.; Gauvreau, Danny; Moore, Jeffrey C.; Hughes, Greg; Devine, Paul N.; O'Shea, Paul D.; Campeau, Louis-Charles
Organic Process Research and Development, 2013 , vol. 17, # 1 p. 61 - 68
反应条件
in toluene T=20°C; 12 h; Heating / reflux;
参考文献
US6664255 B1, ;
Page column 99 ;
US 6664255 B1
反应条件
1: 1) aq. sulfuric acid, NaNO2, 2) KI / 1) 5 deg C, 2) water, at last 80 deg C, 1h 2: 95 percent / conc. sulfuric acid / 5 h / Heating View Scheme
参考文献
Journal of Organic Chemistry, , vol. 55, # 7 p. 2064 - 2069
反应条件
1: triethylamine; palladium diacetate; tris-(o-tolyl)phosphine / 2-methyl tetrahydrofuran / 1 h / 60 - 77 °C / |Inert atmosphere; |Large scale 2: sodium carbonate; dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II) dichloromethane adduct / water; 2-methyl tetrahydrofuran / 16 h / 74 °C / |Inert atmosphere; |Large scale View Scheme
参考文献
Girardin, Melina; Ouellet, Stephane G.; Gauvreau, Danny; Moore, Jeffrey C.; Hughes, Greg; Devine, Paul N.; O'Shea, Paul D.; Campeau, Louis-Charles
Organic Process Research and Development, 2013 , vol. 17, # 1 p. 61 - 68
反应条件
1: triethylamine; palladium diacetate; tris-(o-tolyl)phosphine / 2-methyl tetrahydrofuran / 1 h / 60 - 77 °C / |Inert atmosphere; |Large scale 2: sodium carbonate; dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II) dichloromethane adduct / water; 2-methyl tetrahydrofuran / 16 h / 74 °C / |Inert atmosphere; |Large scale 3: sodium hydroxide / water; 2-methyl tetrahydrofuran / 1.5 h / 72 °C / |Large scale 4: N-ethyl-N,N-diisopropylamine; 1-propanephosphonic acid cyclic anhydride / dichloromethane / 18 h / 12 - 44 °C / |Large scale View Scheme
参考文献
Girardin, Melina; Ouellet, Stephane G.; Gauvreau, Danny; Moore, Jeffrey C.; Hughes, Greg; Devine, Paul N.; O'Shea, Paul D.; Campeau, Louis-Charles
Organic Process Research and Development, 2013 , vol. 17, # 1 p. 61 - 68
反应条件
potassium iodide; nickel dichloride; zinc in N,N,N',N',N'',N''-hexamethylphosphoric triamide T=20°C; 28 h;
参考文献
Takagi, Kentaro; Hayama, Naomi; Inokawa, Saburo
Bulletin of the Chemical Society of Japan, 1980 , vol. 53, # 12 p. 3691 - 3695
反应条件
1: triethylamine; palladium diacetate; tris-(o-tolyl)phosphine / 2-methyl tetrahydrofuran / 1 h / 60 - 77 °C / |Inert atmosphere; |Large scale 2: sodium carbonate; dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II) dichloromethane adduct / water; 2-methyl tetrahydrofuran / 16 h / 74 °C / |Inert atmosphere; |Large scale 3: sodium hydroxide / water; 2-methyl tetrahydrofuran / 1.5 h / 72 °C / |Large scale View Scheme
参考文献
Girardin, Melina; Ouellet, Stephane G.; Gauvreau, Danny; Moore, Jeffrey C.; Hughes, Greg; Devine, Paul N.; O'Shea, Paul D.; Campeau, Louis-Charles
Organic Process Research and Development, 2013 , vol. 17, # 1 p. 61 - 68
反应条件
triethylamine; palladium diacetate; tris-(o-tolyl)phosphine in 2-methyl tetrahydrofuran T=11.5 - 77°C; 1.5 h;
参考文献
Girardin, Melina; Ouellet, Stephane G.; Gauvreau, Danny; Moore, Jeffrey C.; Hughes, Greg; Devine, Paul N.; O'Shea, Paul D.; Campeau, Louis-Charles
Organic Process Research and Development, 2013 , vol. 17, # 1 p. 61 - 68
