282 Singhal, Mishra, and Raj
yielded phenylmercuric isothiocyanate (1.20 g) 3b
[16] and triphenyltin isothiocyanate (1.7 g) 3c [16].
tional crystallization, diphenylantimony trichloride
(0.30 g) 8b [12] and diphenyltindichloride (0.26 g)
8c [13] were obtained.
Reaction of Bis(tri-p-tolyltin) Oxide with
Tellurium Tetrachloride
Reaction of Bis(triphenyltin) Oxide with
Antimony Trichloride
To a stirring solution of bis(tri-p-tolyltin) oxide
(3.0 g, 0.005 mol) in diethyl ether (50 mL), a solu-
tion of tellurium tetrachloride (1.34 g, 0.005 mol) in
the same solvent (30 mL) was added slowly. A white
precipitate appeared immediately. The residue was
digested with benzene (100 mL) for 10 h in a soxlet
extractor to leave off white residue of di(p-tolyl)tin
oxide (0.97 g) 5a [13]. The benzene extract on evapo-
ration yielded (p-tolyl)tellurium trichloride (0.92 g)
5b [9] and tri(p-tolyl)tin chloride (1.15) 5c [13].
To a stirring solution of bis(triphenyltin) oxide
(0.71 g, 1.0 mmol) in diethyl ether (100 mL), a
solution of SbCl3 (0.22 g, 1.0 mmol) in the same
solvent (50 mL) was added slowly. A white solid
appeared immediately. The reactants were further
stirred for 6 h and then filtered hot. The white solid
obtained was identified as polymeric diphenyltin ox-
ide (0.26 g) 10a [13]. The filtrate was completely
evaporated to give a viscous solid. It was then treated
with petroleum ether (60–80◦C)/n-hexane mixture
(1:3) (40 mL), concentrated and then cooled. On
fractional crystallization, phenylantimony dichlo-
ride (0.19 g) 10b [18] and triphenyltin chloride
(0.28 g) 10c [12] were isolated.
Reaction of Bis(tricyclohexyltin) Oxide with
Phenyltellurium Trichloride
To a stirring solution of bis(tricyclohexyltin) oxide
(0.75 g, 1.0 mmol) in toluene (40 mL), phenyltel-
lurium trichloride (0.31 g, 1.0 mmol) in toluene
(20 mL) was added slowly and then refluxed for 6 h
at reflux temperature (110◦C).
ACKNOWLEDGMENTS
The authors thank the Director, Regional So-
phisticated Instrumentation Centre, Central Drug
Research Institute, Lucknow, India, for micro-
analytical and IR data.
A
white precipitate was formed immedi-
ately, which was filtered and dried to afford
di(cyclohexyl)tin oxide (0.27 g) 7a [13]. The filtrate
was further reduced to about 10 mL. A white solid
started to appear at room temperature. The solu-
tion was kept under refrigeration overnight. The
white solid was filtered and dried to yield (cyclo-
hexyl)phenyltellurium dichloride (0.28 g) 7b [17].
Afterward, solvent was completely removed and
residue obtained was dissolved in petroleum ether
(60–80◦C). It was then refrigerated to give white crys-
talline solid, which was filtered and dried under vac-
uum to give tri(cyclohexyl)tin chloride (0.34 g) 7c
[13].
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Reaction of Bis(triphenyltin) Oxide
with Antimony Pentachloride
Antimony pentachloride (0.3 g, 1.0 mmol) in sol-
vent diethyl ether (20 mL) was added slowly to a
stirring solution of bis(triphenyltin) oxide (0.71 g,
1.0 mmol) in diethyl ether (30 mL). A white solid
appeared immediately. The contents were stirred
for 2 h at reflux temperature, and then filtered hot.
The white residue was characterized as polymeric
diphenyltin oxide (0.26 g) 8a [13]. The filtrate was
completely evaporated to give a viscous solid. It was
then treated with petroleum ether/n-hexane mixture
(1:3) (40 mL), concentrated and then cooled. On frac-
Heteroatom Chemistry DOI 10.1002/hc