palladium diacetate; triethylamine in 1,4-dioxane under Ar atm.; Schlenk flask charged with Pd(CH3COO)2 and P(C6H11)2(C6H4C6H5); evapd.; filled (Ar); 1,4-dioxane added; stirred for 30 min at room temp.; Et3N added; soln. of bromoindole in dioxane added; neat pinacolborane added; stirred at 80°C; cooled to room temp.; Celite and activated charcoal added; stirred for 15 min; filtered; solvent removed (vac.); residue diluted (cyclohexane); filtered through a short pad of neutral alumina; purified by column chromy (SiO2, cyclohexane/ethyl acetate);
参考文献
Stadlwieser, Josef F.; Dambaur, Markus E.
Helvetica Chimica Acta, 2006 , vol. 89, # 5 p. 936 - 946
(CF3SO2)2NLi in tetrahydrofuran Electrolysis; electrolysis (2-6 F/mol) with Mg anode under inert atm. at room temp. at0.15 A/dm**2; after electrolysis, solvent evapd. under vac.; slowly hyd rolysed at 0°C with soln. of H2SO4 until pH 5; purified by column chromy. on silica gel (pentane/ether);
triethylamine; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; triphenyl-arsane in 1,4-dioxane T=80°C; Borylation; 16 h; Title compound not separated from byproducts;
triethylamine; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; triphenyl-arsane in 1,4-dioxane T=80°C; Borylation; 16 h; Title compound not separated from byproducts;
1: With lithium bis((trifluoromethyl)sulfonyl)amide in tetrahydrofuran T=20°C; Electrochemical reaction; 2: With sulfuric acid T=0°C; pH=5; Further stages.;
参考文献
Laza, Carine; Dunach, Elisabet
Advanced Synthesis and Catalysis, 2003 , vol. 345, # 5 p. 580 - 583
