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A solution of the crude 2,3-Benzbromarone in ethanol (10 ml) was added dropwise under nitrogen to a stirred ice-cold solution of Ethylamine gas (10.0 g, 0.32 mole) in ethanol (130 ml) during 50 min, and the mixture was stirred a t 0" 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 ether and evaporated to dryness. The yellow solid was extracted with chloroform (4 X 50 ml), and the re- sidual Ethylamine hydrochloride was discarded. Evaporation of the chloroform filtrates gave an off-white solid, which was recrystallized twice from ethanol-acetone to give 3.4 g (17%) of 2,3-Bzrone hydrochlo- ride as off-white crystals, mp 117-119' [lit. (21) mp 116-117']; TLC in chloro-form-2-propanol-triethylamine (62:35:3) showed a single spot, Rf 0.55. ·Ç³£¸Ðл£¡ |
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flame95
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- ½ð±Ò: 3049.9
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- ×¢²á: 2008-09-19
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Mally89: ½ð±Ò+1 2012-04-14 13:34:43
sltmac: ½ð±Ò+30, ·ÒëEPI+1 2012-04-19 10:13:20
Mally89: ½ð±Ò+1 2012-04-14 13:34:43
sltmac: ½ð±Ò+30, ·ÒëEPI+1 2012-04-19 10:13:20
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