1: tBuCH2CH2B(H)NiPr2; 3-bromobenzenediazonium tetrafluoroborate With biscyclopentadienyliron(II) in acetonitrile
T=20°C; 2.5 h;
2: With methanol in acetonitrile
T=0 - 20°C; 1 h;
3: 2,3-dimethylbutane-2,3-diol in diethyl ether; acetonitrile
T=20°C; 4 h; Reagent/catalyst;
参考文献
UNIVERSITE DE BORDEAUX 1; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; PUCHEAULT, Mathieu Jonathan Damien; MARCIASINI, Ludovic Daniel Alain; VAULTIER, Michel
Patent: WO2014/9169 A1, 2014 ;
Location in patent: Page/Page column 63-64 ;
copper(l) iodide; iron (III) acetylacetonate; N,N,N',N,-tetramethylethylenediamine; sodium hydride in tetrahydrofuran; mineral oil
T=-10°C; Inert atmosphere;
参考文献
Labre, Flavien; Gimbert, Yves; Bannwarth, Pierre; Olivero, Sandra; Dunach, Elisabet; Chavant, Pierre Y.
Organic Letters, 2014 , vol. 16, # 9 p. 2366 - 2369
(CF3SO2)2NLi in tetrahydrofuran
Electrolysis; electrolysis (1 F/mol) with Mg anode under inert atm. at room temp. at 0.15 A/dm**2; after electrolysis, solvent evapd. under vac.; slowly hydrolysed at 0°C with soln. of H2SO4 until pH 5; purified by column chromy. on silica gel (pentane/ether);
