Technology Process of 1-(4-nitrophenyl)-1,7-dicarba-closo-dodecaborane(12)
There total 2 articles about 1-(4-nitrophenyl)-1,7-dicarba-closo-dodecaborane(12) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
n-butyllithium; copper(l) chloride;
In
tetrahydrofuran; diethyl ether; hexane;
under N2; dropwise addn. of BuLi in hexane to a soln. of m-carborane inether at 0-5°C with stirring; addn. of anhydr. CuCl with stirring; addn. of THF; heating at 40°C for 10 min; cooling to 0-5°C; addn. of BF4-salt; addn. of MeOH at 20°C; filtration of ppt. and washing (benzene, ether); washing of filtrates (aq. HCl, H2O) and drying over CaCl2 or Na2SO4; evapn. in vac.; TLC (Siloful, benzene-petroleum ether); recrystn. (EtOH); elem. anal.;
- Guidance literature:
-
With
pyridine; n-butyllithium; copper(l) chloride;
In
1,2-dimethoxyethane; hexane;
under N2; BuLi/hexane is added dropwise to stirred carborane/DME, stirred at r. t. (15 min), CuCl is added (ratio carborane:CuCl 1:2), stirred (15 min, r. t.), pyridine is added, the aryl iodide is added, heated and stirred (95°C, 90 h); cooled, allowed to stand for 2 h (or more), filtd., the filtrate is evapd., the residue is chromd., elem. anal.;
DOI:10.1016/0022-328X(93)83337-U
- Guidance literature:
-
In
tetrahydrofuran;
stirring (45 min, 25°C); dichloromethane addn., washing (water, three times), layers sepn., dichloromethane layer drying (MgSO4), solvent evapn., recrystn. (ethanol); elem. anal.;
DOI:10.1016/0277-5387(95)00297-6
