Technology Process of 1,2-bis(dimethylstibanylmethyl)benzene
There total 3 articles about 1,2-bis(dimethylstibanylmethyl)benzene which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
Mg; 1,2-dibromethane;
In
toluene;
(N2); activation of Mg powder with 1,2-dibromoethane in THF; addn. of THF; addn. dropwise of C6H4(CH2Cl2)2; after 15 h, treatment dropwise with soln. of Me2SbCl in toluene; stirring overnight; addn. of aq. NH4Cl; sepn. of org. layer; washing of aq. layer with Et2O;drying of combined organics over anhyd. MgSO4; removal of solvent in va c., as oil;
DOI:10.1039/b312083j
- Guidance literature:
-
With
aq. NH4Cl;
In
tetrahydrofuran; toluene;
byproducts: Sb2Me4; under N2; to soln. of C6H4(CH2MgCl)2 in THF was added soln. of Me2SbCl in toluene over 30 min, mixt. left to stir overnight, mixt. was then hydrolysed with aq. NH4Cl; organics sepd., aq. layer extd. with Et2O, after drying (MgSO4), filtering, removing the solvent by distillation at atm. pressure, fractionationof C6H4(CH2SbMe2)2 (200°C, 0.5 mm Hg), oil was obtained by Kugel roehr distillation (225°C, ...;
DOI:10.1039/b610808c
- Guidance literature:
-
In
diethyl ether;
bubbling of HCl through soln. of PhMe2Sb in toluene for 15 min, purging with N2; addn. of sodium in liquid ammonia at -78°C; stirring for2 h; addn. dropwise of C6H4(CH2Br)2 in Et2O; warming to room temp., addn. of aq. NH4Cl; sepn. of org. layer; washing of aq. layer with Et2O; drying of combined organics over anhyd. MgSO4; removal of solvent in vac., Kugelroehr distn. at 200°C (0.5 mm Hg);
DOI:10.1039/b312083j