EFIMOVA et al.
154
acid in 5 ml of 17.5% aqueous hydrogen peroxide. The
mixture was stirred for 45 min at 50°C (20 W) in
a microwave furnace, cooled to 20°C, and diluted with
15 ml of cold water. The precipitate was filtered off,
washed with water, and dried in air. The filtrate was
neutralized to pH 7 with 25% aqueous ammonia and
extracted with chloroform (3×10 ml). The extracts
were combined and evaporated under reduced pres-
sure, and the residue was combined with the precip-
itate. Yield 77%, mp 70°C (from petroleum ether) [9].
IR spectrum, ν, cm–1: 3424, 3130, 3109, 3020, 2971,
2940, 2838, 1613, 1594, 1499, 1490, 1460, 1386,
1316, 1285, 1244, 1202, 1177, 1164, 1095, 1089,
1058, 1049, 1039, 1007, 962, 853, 770, 683, 572.
1H NMR spectrum (CDCl3), δ, ppm: 3.90 s (3H,
OCH3), 7.04–7.07 d (1H, Harom), 7.26–7.29 m (2H,
Harom), 7.46–7.50 t (1H, Harom), 8.97 s (1H, 5-H).
checked by TLC on Silufol plates using acetone–
hexane (1:2) as eluent.
This study was performed under financial support
by the Russian Foundation for Basic Research (project
no. 08-03-00342a).
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RUSSIAN JOURNAL OF ORGANIC CHEMISTRY Vol. 46 No. 1 2010