(4-氯-2-氟苯基)(6-氯-2-甲基-8-(吗啉甲基)咪唑并[1,2- b]吡嗪-3-基)甲酮合成路线 (共 6 条)
反应条件
bis(acetylacetonate)oxovanadium in ethanol T=23 - 40°C; 50.5 h; Inert atmosphere; Product distribution / selectivity;
参考文献
ELI LILLY AND COMPANY
Patent: US2010/152181 A1, 2010 ;
Location in patent: Page/Page column 4 ;
反应条件
potassium carbonate in water T=120°C; 0.333333 h; Microwave irradiationSealed tube; Product distribution / selectivity;
参考文献
ELI LILLY AND COMPANY
Patent: US2010/152181 A1, 2010 ;
Location in patent: Page/Page column 4 ;
反应条件
bis(acetylacetonate)oxovanadium in ethanol T=30 - 40°C; 26.5 h; Large scale reaction;
参考文献
Mitchell, David; Cole, Kevin P.; Pollock, Patrick M.; Coppert, David M.; Burkholder, Timothy P.; Clayton, Joshua R.
Organic Process Research and Development, 2012 , vol. 16, # 1 p. 70 - 81
反应条件
1: sodium bromide / N,N-dimethyl-formamide / 30 h / 35 °C / Inert atmosphere; Large scale reaction 2: bis(acetylacetonate)oxovanadium / ethanol / 26.5 h / 30 - 40 °C / Large scale reaction View Scheme
参考文献
Mitchell, David; Cole, Kevin P.; Pollock, Patrick M.; Coppert, David M.; Burkholder, Timothy P.; Clayton, Joshua R.
Organic Process Research and Development, 2012 , vol. 16, # 1 p. 70 - 81
反应条件
1: sulfuryl dichloride / methanol; dichloromethane / 7 h / -5 - 0 °C / Large scale reaction 2: sodium bromide / N,N-dimethyl-formamide / 30 h / 35 °C / Inert atmosphere; Large scale reaction 3: bis(acetylacetonate)oxovanadium / ethanol / 26.5 h / 30 - 40 °C / Large scale reaction View Scheme
参考文献
Mitchell, David; Cole, Kevin P.; Pollock, Patrick M.; Coppert, David M.; Burkholder, Timothy P.; Clayton, Joshua R.
Organic Process Research and Development, 2012 , vol. 16, # 1 p. 70 - 81
反应条件
1.1: triethylsilane; trifluoroacetic acid / 27 h / 50 - 88 °C / Inert atmosphere; Large scale reaction 1.2: 50 °C / pH 10 - 11 / Large scale reaction 2.1: tris-(dibenzylideneacetone)dipalladium(0); 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene; sodium hydroxide / anhydrous xylene; water / 40 h / Inert atmosphere; Reflux; Large scale reaction 3.1: trifluoroacetic acid / water / 7 h / 95 - 100 °C / Large scale reaction 3.2: 8 h / 60 °C / pH 10 - 11 View Scheme
参考文献
Mitchell, David; Cole, Kevin P.; Pollock, Patrick M.; Coppert, David M.; Burkholder, Timothy P.; Clayton, Joshua R.
Organic Process Research and Development, 2012 , vol. 16, # 1 p. 70 - 81