842
M. S. Singh and P. Singh
calcd. for C15H14N2O2: C, 70.85; H, 5.55; N, 11.02. Found: C, 70.43; H,
5.22; N, 10.81.
Synthesis of Dibenzodioxadiazasilaundecine [1]
To a stirred suspension of NaH (96 mg, 4 mmoles) in dry dioxane (5 mL)
was added dioxane solution (55 mL) of ligand I (508 mg, 2 mmoles) drop-
wise with constant stirring and, it was refluxed for 4 h in an inert atmo-
sphere. Thus the yellowish brown solution of dianion generated in situ
was cooled to r.t. dichlorodimethylsilane (258 mg, 2 mmoles) was added
dropwise with constant stirring, and the reaction mixture was refluxed
for an additional 5 h. Completion of the reaction was checked by TLC.
The reaction mixture was evaporated with the help of a rotary evapora-
tor, and the residue obtained was subjected to solumn chromatography
(n-hexane/ethyl acetate, 8:1) to give 1. All other silaheterocycles (2–8)
were also synthesized analogously as previously described in the de-
sired molar ratios. The analytical and spectral data for compounds 1 to
8 are listed in Tables I and II, respectively.
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