(CF3SO2)2NLi in tetrahydrofuran
Electrolysis; electrolysis (2 F/mol) with Mg anode under inert atm. at room temp. at 30 mA; after electrolysis, solvent evapd. under vac.; slowly hydrolysed at 0°C with soln. of H2SO4 until pH 5; further products: C6H3(B(OC(CH3)2C(CH3)2O))2Br; purified by column chromy. on silica gel (pentane/ether);
1: 1,3,5-tribromo benzene With magnesium in tetrahydrofuran
T=20°C; 2 h;
2: benzoyl chloride With bis[2-(N,N-dimethylamino)ethyl] ether in tetrahydrofuran
T=0°C; 4 h;
3: With hydrogenchloride; water
pH=5;
参考文献
TRANSITIONS OPTICAL, INC.
Patent: WO2012/82999 A1, 2012 ;
Location in patent: Page/Page column 37 ;
(CF3SO2)2NLi in tetrahydrofuran
Electrolysis; electrolysis (2 F/mol) with Mg anode under inert atm. at room temp. at 30 mA; after electrolysis, solvent evapd. under vac.; slowly hydrolysed at 0°C with soln. of H2SO4 until pH 5; further products: C6H3(B(OC(CH3)2C(CH3)2O))2Br; purified by column chromy. on silica gel (pentane/ether);
