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| A solution of the ÔÁÏ in ¼×´¼ (10 ml) was added dropwise under nitrogen to a stirred ice-cold solution of ¶þÒÒ°· (10.0 g, 0.32 mole) in ¼×´¼ (130 ml) during 50 min, and the mixture was stirred at 0¡ãC for an additional 40 min. A mixture of 12 N HCl (30 ml) and ice was added to pH < 7, and the aqueous solution was extracted with ÒÒÃÑ and evaporated to dryness. The yellow solid was extracted with ÂÈ·Â (4 X 50 ml), and the re-sidual ¶þÒÒ°·ÑÎËáÑÎ was discarded. Evaporation of the ÂÈ·Â filtrates gave an off-white solid, which was recrystallized twice from ÒÒ´¼-±ûͪ to give 3.41 g (17.1%) of ²úÎï as off-white crystals, mp 76-79¡ãC. |
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