1-甲基-3-(4,4,5,5-四甲基-1,3,2-二噁硼烷-2-基)-1H-吲哚合成路线 (共 10 条)
反应条件
1: 1-methyl-1H-indole; chlorocatecholborane With AlCl3, aluminium chloride; triethylamine in dichloromethane
T=20°C; 6 h; Inert atmosphere;
2: 2,3-dimethylbutane-2,3-diol With triethylamine in dichloromethane
Irradiation;
参考文献
THE UNIVERSITY OF MANCHESTER; INGLESON, Michael James
Patent: WO2012/25760 A1, 2012 ;
Location in patent: Page/Page column 54-55 ;
反应条件
1: 1-methyl-1H-indole With 2,6-dimethylpyridine; AlCl3, aluminium chloride; boron trichloride in n-heptane; dichloromethane
T=20°C; 14 h; Inert atmosphere;
2: 2,3-dimethylbutane-2,3-diol With triethylamine in n-heptane; dichloromethane
T=20°C; 0.5 h; Irradiation;
参考文献
THE UNIVERSITY OF MANCHESTER; INGLESON, Michael James
Patent: WO2012/25760 A1, 2012 ;
Location in patent: Page/Page column 45-46 ;
反应条件
Et3N in dichloromethane
byproducts: Et3NH-AlCl4; to borenium cation made in situ (in Schlenk, to soln. Et2N (CH2Cl2) added CatBCl, AlCl3; stirred) at 20°C arene added (CH2Cl2); excess Et3N added; pinacol added; stirred for 4 h;; (11)B (1H) NMR; volatiless remowed under vac; extracted (hexane); filtered through silica; removal of solvent;;
参考文献
Del Grosso, Alessandro; Singleton, Paul J.; Muryn, Christopher A.; Ingleson, Michael J.
Angewandte Chemie - International Edition, 2011 , vol. 50, # 9 p. 2102 - 2106
反应条件
AlCl3; 2,6-lutidine in dichloromethane
1:1 mixt. of BCl3 and AlCl, pinacol (2.3-3.0 equiv.) and lutidine (15 equiv.) for 14 h;
参考文献
Del Grosso, Alessandro; Helm, Matthew D.; Solomon, Sophia A.; Caras-Quintero, Dolores; Ingleson, Michael J.
Chemical Communications, 2011 , vol. 47, # 46 p. 12459 - 12461
反应条件
C32H12BF24(1-)*C42H38F3PRuS(1+)
T=80°C; 24 h; GloveboxSealed tubeInert atmosphere; SolventReagent/catalyst;
参考文献
Stahl, Timo; Muether, Kristine; Ohki, Yasuhiro; Tatsumi, Kazuyuki; Oestreich, Martin
Journal of the American Chemical Society, 2013 , vol. 135, # 30 p. 10978 - 10981
反应条件
triethylamine in dichloromethane
T=20°C; 1.25 h; Inert atmosphere;
参考文献
Del Grosso, Alessandro; Helm, Matthew D.; Solomon, Sophia A.; Caras-Quintero, Dolores; Ingleson, Michael J.
Chemical Communications, 2011 , vol. 47, # 46 p. 12459 - 12461
反应条件
1.1: AlCl3, aluminium chloride; triethylamine / dichloromethane / 20 °C / Inert atmosphere
1.2: 4 h / 20 °C / Inert atmosphere
2.1: triethylamine / dichloromethane / 1 h / Inert atmosphere
View Scheme
参考文献
Del Grosso, Alessandro; Singleton, Paul J.; Muryn, Christopher A.; Ingleson, Michael J.
Angewandte Chemie - International Edition, 2011 , vol. 50, # 9 p. 2102 - 2106
反应条件
C22H34CoN3 in neat (no solvent)
T=80°C; 24 h; Inert atmosphereGlovebox;
参考文献
Obligacion, Jennifer V.; Semproni, Scott P.; Chirik, Paul J.
Journal of the American Chemical Society, 2014 , vol. 136, # 11 p. 4133 - 4136
反应条件
1.1: sodium hydride / N,N-dimethyl-formamide / 1 h / 20 °C / |Inert atmosphere; |Schlenk technique
1.2: 20 °C
2.1: C32H12BF24(1-)*C42H38F3PRuS(1+) / 24 h / 80 °C / |Glovebox; |Sealed tube; |Inert atmosphere
View Scheme
参考文献
Stahl, Timo; Muether, Kristine; Ohki, Yasuhiro; Tatsumi, Kazuyuki; Oestreich, Martin
Journal of the American Chemical Society, 2013 , vol. 135, # 30 p. 10978 - 10981
反应条件
in dichloromethane; dichloromethane-d2
using standard Schlenk techniques; Et3N in CD2Cl2-CH2Cl2 treated with B compd. and AlCl3; treated with N-methylindole for 3 h; treated with Et3Nand pinacol; rotated for 30 min; solvent removed under vac.; dried for 1 h; hexane added; filtered; hexane removed from filtrate under vac.; dried overnight; monitored by (1)H and (11)B NMR spectra;
参考文献
Solomon; Del Grosso; Clark; Bagutski; McDouall; Ingleson
Organometallics, 2012 , vol. 31, # 5 p. 1908 - 1916