Andrey V. Gutnov
North-Ossetian State University, RUS-362040 Vladikavkaz, Russian
Federation.
Fax: +7 867 227 3216, E-mail: [email protected]
Received: 22 September 1997 / Published: 1 October 1997
See also [1,2]. To the solution of 2-bromobenzaldehyde (18.5 g, 100 mmol) and sylvan (20 ml, 250 mmol) in 100 ml of benzene 5 ml of Me3SiCl was added at room temperature. The mixture warmed up to 50-60deg.C within 15 min and a water layer separated. After standing for an additional 1 hr, the organic layer was washed with NaHCO3 solution, separated from the water layer and evaporated. The residue was recrystallised from hexane. Yield 29 g (87.7%) of colourless cubes.
M.p. 56-57deg.C.
1H-NMR (CDCl3): 7.54-7.01 (m, 4H, HAr), 5.82-5.73 (q, 4H, 3,4-HFur), 5.73 (s, 1H, CH), 2.16 (s, 6H, CH3) ppm.
Anal. calc. for C17H15BrO2 (331.2): C 61.65, H 4.56, Br 24.13; found: C 61.7, H 4.5, Br 24.0.
Acknowledgment: The author would like to thank Mr. Vladimir Ch. Gutnov and Mrs. Vera N. Gutnova for financial support of his activity.
References and Notes
1. Gutnov, A. V.; Abaev, V. T.; Butin, A. V.; Zavodnik, V. E.; Kul'nevich, V. G. Khim. Geterotsikl. Soedin. 1996, 12, 162-167.
2. Jones, G.; McKinley, W. H. J. Chem. Soc. Perkin Trans. 1. 1979. 599.
Sample availability: 2.5 g.
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