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495829488銅蟲 (小有名氣)
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[求助]
2-溴二苯并呋喃合成
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求助2-溴二苯并呋喃合成路線,用溴素溴化二苯并呋喃,二取代較多且不易純化 , |
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參見Journal of Organic Chemistry, 1997, vol. 62, # 5, p. 1348 - 1355 ,溴取代得到就是一個混合物。 6% dibenzofuran, 82.5%1, 0.4% of another monobromo compound, and 11% of a dibromo compound (GC, DB-5, 200 °C: tR 2.66, 4.90, 4.73, and11.02 min, respectively). 參見Journal of the American Chemical Society, 2022, vol. 144, # 14, p. 6551 - 6557 ,2-Bromodibenzofuran: Dibenzofuran (1.68 g, 10 mmol)) and Br2 (0.56 mL, 11mmol) were dissolved in chloroform (20 mL) and stirred for 24 h at room temperature. Then, the solvent was removed by rotary evaporation. The resulted white solid was further purified by recrystallization from dichloromethane/methanol to afford whitecrystal (1.98 g) with a yield of 80%. 1 ,如果樓主就打算從溴素溴化二苯并呋喃,反應(yīng)時降低下溴素的當量和反應(yīng)溫度提高選擇性,還有嘗試二氯甲烷:甲醇重結(jié)晶提純目標產(chǎn)物。 用NBS作為溴代試劑估計二溴代會少些,不過可能原料剩的多些。 |
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