4,5-双二苯基膦-9,9-二甲基氧杂蒽合成路线 (共 16 条)
反应条件
1: 9,9-dimethyl-9H-xanthene With N,N,N',N,-tetramethylethylenediamine; sec.-butyllithium in tert-butyl methyl ether; cyclohexane T=6 - 10°C; 2: in cyclohexane; water T=20°C; 14 h; 3: chloro-diphenylphosphine in cyclohexane; water T=10 - 20°C; 5.16667 h;
参考文献
Zhao, Matthew M.; Yin, Jingjun
Patent: US2004/23979 A1, 2004 ;
Location in patent: Page/Page column 9; 10 ;
US 20040023979 A1
反应条件
1: With bis 1,2-(dimethylamino)ethylene; sec.-butyllithium in tert-butyl methyl ether T=10 - 20°C; 16 h; 2: With chloro-diphenylphosphine T=20°C; 6.25 h;
参考文献
US2004/23980 A1, ;
Page/Page column 15 ;
反应条件
1: phenyllithium With DABCO-bis(sulfur dioxide) in 1,4-dioxane T=20°C; 2 h; Inert atmosphereSchlenk technique; 2: bromobenzene; 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene With palladium diacetate; caesium carbonate T=85°C; 16 h; Inert atmosphereSchlenk technique;
参考文献
Emmett, Edward J.; Hayter, Barry R.; Willis, Michael C.
Angewandte Chemie - International Edition, 2013 , vol. 52, # 48 p. 12679 - 12683
Angew. Chem., 2013 , vol. 125, # 48 p. 12911 - 12915,5
反应条件
1: phenyllithium With DABCO-bis(sulfur dioxide) in 1,4-dioxane T=20°C; 2 h; Inert atmosphereSchlenk technique; 2: 1-(iodo)-4-methylbenzene; 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene With palladium diacetate; caesium carbonate T=70°C; 16 h; Inert atmosphereSchlenk technique; Reagent/catalystTemperature;
参考文献
Emmett, Edward J.; Hayter, Barry R.; Willis, Michael C.
Angewandte Chemie - International Edition, 2013 , vol. 52, # 48 p. 12679 - 12683
Angew. Chem., 2013 , vol. 125, # 48 p. 12911 - 12915,5
反应条件
in tetrahydrofuran N2 atmosphere, stirring (room temp., overnight); removement of solvent (vacuum), washing (Et2O), drying (vacuum);
参考文献
European Journal of Inorganic Chemistry, , # 2 p. 155 - 157
反应条件
in dichloromethane; acetonitrile solns. of PdCl2 in MeCN and phosphorous ligand in CH2Cl2 mixed together,stirred (30 min. room temp.); solvent removed (reduced pressure), washed (Et2O), recrystd. (CH2Cl2 andhexane); elem. anal., XRD;
参考文献
Journal of Organometallic Chemistry, , vol. 696, # 26 p. 4293 - 4297
反应条件
potassium phosphate; tris(dibenzylideneacetone)dipalladium (0) in 1,4-dioxane T=100°C;
参考文献
Yin, Jingjun; Zhao, Matthew M.; Huffman, Mark A.; McNamara, James M.
Organic Letters, 2002 , vol. 4, # 20 p. 3481 - 3484
反应条件
1: phenyllithium With DABCO-bis(sulfur dioxide) in 1,4-dioxane T=20°C; 2 h; Inert atmosphereSchlenk technique; 2: bromobenzene; 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene With palladium diacetate; caesium carbonate T=85°C; 16 h; Inert atmosphereSchlenk technique;
参考文献
Emmett, Edward J.; Hayter, Barry R.; Willis, Michael C.
Angewandte Chemie - International Edition, 2013 , vol. 52, # 48 p. 12679 - 12683
Angew. Chem., 2013 , vol. 125, # 48 p. 12911 - 12915,5
反应条件
1: phenyllithium With DABCO-bis(sulfur dioxide) in 1,4-dioxane T=20°C; 2 h; Inert atmosphereSchlenk technique; 2: 1-(iodo)-4-methylbenzene; 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene With palladium diacetate; caesium carbonate T=70°C; 16 h; Inert atmosphereSchlenk technique; Reagent/catalystTemperature;
参考文献
Emmett, Edward J.; Hayter, Barry R.; Willis, Michael C.
Angewandte Chemie - International Edition, 2013 , vol. 52, # 48 p. 12679 - 12683
Angew. Chem., 2013 , vol. 125, # 48 p. 12911 - 12915,5
反应条件
1,2,4,5-tetramethyl benzene; caesium carbonate; tris(dibenzylideneacetone)dipalladium(0) chloroform complex in 1,4-dioxane
T=100°C; 10 h;
参考文献
Sergeev; Artamkina; Beletskaya
Russian Journal of Organic Chemistry, 2003 , vol. 39, # 12 p. 1741 - 1752