至尊木虫 (职业作家)
皇家神龙教---九月风
|
【答案】应助回帖
★ ★ 495829488(wolfghost代发): 金币+2, 有效应助奖励~ 2022-10-11 19:45:23 wolfghost: 博学EPI+1 2022-10-11 19:45:27
参见Journal of Organic Chemistry, 1997, vol. 62, # 5, p. 1348 - 1355 ,溴取代得到就是一个混合物。
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).
参见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 ,如果楼主就打算从溴素溴化二苯并呋喃,反应时降低下溴素的当量和反应温度提高选择性,还有尝试二氯甲烷:甲醇重结晶提纯目标产物。
用NBS作为溴代试剂估计二溴代会少些,不过可能原料剩的多些。 |
|