2-羟基-5-碘-3-三氟甲基吡啶合成路线 （共 7 条）
反应条件
N-iodo-succinimide; acetic acid in acetonitrile T=65°C; 5 h; Industrial scale;
参考文献
Cleator, Ed; Scott, Jeremy P.; Avalle, Paulo; Bio, Matthew M.; Brewer, Sarah E.; Davies, Antony J.; Gibb, Andrew D.; Sheen, Faye J.; Stewart, Gavin W.; Wallace, Debra J.; Wilson., Robert D.
Organic Process Research and Development, 2013 , vol. 17, # 12 p. 1561 - 1567
反应条件
1: 73 percent / KOH / 2-methyl-propan-2-ol / 10 h / Heating 2: potassium carbonate; iodine / H2O / 13 h / 20 - 50 °C View Scheme
参考文献
Synthetic Communications, , vol. 36, # 9 p. 1235 - 1245
反应条件
trichlorophosphate in N,N-dimethyl-formamide T=110°C; 0.333333 h; Microwave irradiation;
参考文献
SLOAN-KETTERING INSTITUTE FOR CANCER RESEARCH
Patent: WO2008/119015 A2, 2008 ;
Location in patent: Page/Page column 48-49 ;
反应条件
silver carbonate in tetrahydrofuran; hexane
T=40°C; 25 h;
参考文献
Kagabu, Shinzo
Synthetic Communications, 2006 , vol. 36, # 9 p. 1235 - 1245
反应条件
1: 920 mg / silver(I) carbonate / hexane; tetrahydrofuran / 25 h / 40 °C
2: 82 percent / tetrakis(triphenylphosphine)palladium(0) / dimethylformamide / 8 h / 80 °C
View Scheme
参考文献
Kagabu, Shinzo
Synthetic Communications, 2006 , vol. 36, # 9 p. 1235 - 1245
反应条件
1.1: 920 mg / silver(I) carbonate / hexane; tetrahydrofuran / 25 h / 40 °C
2.1: 82 percent / tetrakis(triphenylphosphine)palladium(0) / dimethylformamide / 8 h / 80 °C
3.1: diisobutyl aluminum hydride / toluene / 12 h / 20 °C
3.2: 43 percent / sodium borohydride / methanol / 12 h / 20 °C
4.1: 66 percent / POCl3 / dimethylformamide / 0.67 h / 100 °C
View Scheme
参考文献
Kagabu, Shinzo
Synthetic Communications, 2006 , vol. 36, # 9 p. 1235 - 1245
反应条件
1: trichlorophosphate / N,N-dimethyl-formamide / 4 h / 110 °C
2: sodium t-butanolate / 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene; tris-(dibenzylideneacetone)dipalladium(0) / toluene / 2 h / Inert atmosphere; Reflux
3: 1,1'-bis-(diphenylphosphino)ferrocene; tris-(dibenzylideneacetone)dipalladium(0) / N,N-dimethyl-formamide / 0.5 h / 170 °C / Reflux; Inert atmosphere
4: trifluoroacetic acid / dichloromethane / 3 h / 20 °C
View Scheme
参考文献
ARAGON PHARMACEUTICALS, INC.; SMITH, Nicholas, D.; BONNEFOUS, Celine; JULIEN, Jackaline, D.
Patent: WO2011/103202 A2, 2011 ;
WO 2011/103202 A2
