Technology Process of 9-benzyl-1,2-carborane
There total 3 articles about 9-benzyl-1,2-carborane which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
((C6H5)3P)2PdCl2 or ((C6H5)3P)4Pd;
In
diethyl ether;
refluxed for 25-30 h, inert atm.; addition of water, washing an ether soln. with aq. HCl, water, drying with CaCl2, column chromy. (silica gel, benzene-petroleum ether, 15:85), sublimation (100-120°C, 1 torr), recrystn. (hexane); elem. anal.;
DOI:10.1016/S0022-328X(00)83405-1
- Guidance literature:
-
With
zinc(II) chloride;
tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran; diethyl ether;
ether soln. of Grignard compd. addn. to THF soln. of Zn-compd., stirring(Ar atmosphere, 20°C, 30-40 min), addn. of THF soln. of Pd-compd . and iodoborane, heating and refluxing (20-30 h); mixture cooling, pouring to aq. HCl, organic layer extracting (Et2O), drying (Na2SO4), solvent removing (vacuum), residue purification by columnchromy. (silica gel/benzene-petroleum ether), residue re-crystn. or vac uum distillation; melting point;
- Guidance literature:
-
With
potassium carbonate;
In
diethyl ether; acetone;
at 40 ℃;
for 12h;
Inert atmosphere;
Schlenk technique;
DOI:10.1021/jacs.8b10270