222
BASENKO et al.
Reactions with other alcohols were carried out in
REFERENCES
similar manner (see the table for NMR parameters).
1. Sommer, L.H., Stereochemistry, Mechanism, and Siliꢀ
con, New York: McGrawꢀHill, 1965. Translated under
the title Stereokhimiya i mekhanizmy reaktsii kremniiorꢀ
ganicheskikh soedinenii, Moscow: Mir, 1966.
Phenyl(trimethylsilylamino)fluorochlorosilane
PhSiFCl(NHSiMe3). A mixture of 1.80 g (0.01 mol) of
phenyl(fluoro)dichlorosilane and 1.61 g (0.01 mol) of
hexamethyldisilazane was kept at ambient temperaꢀ
ture for 5 min. After trimethylchlorosilane (0.9 g,
2. Corriu, R.J.P., Guerin, C., and Moreau, J.J.E., The
Chemistry of Organic Silicon Compounds, New York:
Wiley, 1989, vol. 1, p. 305.
98%) with bp 57
distilled in vacuum to give 2.10 g (91.0%) of
PhSiFCl(NHSiMe3), bp 71–71.5 C (2 mmHg).
°
C was distilled off, the residue was
3. Kawachi, A., Maeda, H., Mitsudo, K., and Tamao, K.,
°
Organometallics, 1999, vol. 18, p. 4350.
19F NMR (
, ppm): –122.26.
29Si NMR (
, ppm): –26.1 (d, PhSi
289.9 Hz), 6.9 (–SiMe3).
δ
4. Bohme, U., Wiesner, S., and Gunther, B., Inorg. Chem.
Commun., 2006, vol. 9, no. 8, p. 806.
δ
≡, JSi–F =
5. Ishikawa, N. and Kuroda, K., Kogyo Kagaku Zasshi
,
1969, vol. 72, no. 12, p. 2602. (Chem. Abstr., 1970,
The reactions of phenyl(fluoro)dichlorosilane with
hexamethyldisiloxane, octamethyltrisiloxane, trimeꢀ
thylacyloxysilanes, and carboxylic acid anhydrides
were carried out in similar manner. The hydrolysis of
PhSiFCl2 and its cohydrolysis with phenyldifluoroꢀ
chlorosilane and phenyltrichlorosilane were conꢀ
ducted by passing atmospheric air through the
reagents. The composition and structure of the
obtained compounds were confirmed by 19F and 29Si
NMR spectra and corresponding 19F–29Si spin–spin
coupling constants (table). The IR spectra showed the
absorption bands of all functional groups of the preꢀ
pared compounds.
vol. 72, 100813x).
6. Kunai, A., Sakurai, T., Toyoda, E., and Ishikawa, M.,
Organometallics, 1996, vol. 15, no. 10, p. 2478.
7. Vainshtein, B.I. and Vaks, E.A., Zh. Org. Khim., 1976,
vol. 46, no. 9, p. 2052.
8. Vaks, E.A. and Vainshtein, B.I., Zh. Org. Khim., 1977,
vol. 47, no. 4, p.782.
9. Albanov, A.I., Gubanova, L.I., Larin, M.F., et al.,
J. Organomet. Chem., 1983, vol. 244, no. 1, p. 5.
10. Kuroda, K. and Ishikawa, N., Kogyo Kagaku Zasshi.
1971, vol. 74, no. 10, p. 2132. (Chem. Abstr., 1972,
vol. 76, 60125Y).
,
DOKLADY CHEMISTRY Vol. 439
Part 2
2011