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nirenjie0627金蟲 (小有名氣)
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稱取一縮二乙二醇63.6g置于四口燒瓶中,量取PBr348ml于恒壓滴液漏斗中,裝上冷凝管、尾氣吸收以及攪拌裝置,開啟加熱電源,將PBr3緩慢滴加至四口燒瓶中,2h滴完,控制反應(yīng)溫度為90℃,繼續(xù)回流反應(yīng)6h。反應(yīng)產(chǎn)物用10% NaHCO3溶液、蒸餾水各洗3次,在分出的有機相中加入1.5g無水硫酸鎂,攪拌2min,靜置30min,過濾得到1-溴-2-(2-溴乙氧基)乙烷中間體125.8g,收率為90.4%(以一縮二乙二醇量計),保存?zhèn)溆谩? |
鐵桿木蟲 (知名作家)
帝國空軍中將
| Weigh 63.6g of diethylene glycol and put it in four flasks. Take 348ml of PBr into the constant pressure dropping funnel, turn on the heating power after installing condenser, off-gas absorption and mixing device, and then drop slowly PBr3 into the four flasks with 2 hours controlling the reaction temperature at 90℃ during this process, continuing reflux reaction within 6 hours. Reaction products are washed with 10% solution of NaHCO3 and distilled water each for 3 times. Add 1.5g of anhydrous magnesium sulfate into the separation of the organic phase, after 2 minutes of stirring and putting aside for 30 minutes, and get 125.8g of 1-bromo-2-(2-bromo ethoxy yl) ethane intermediate by filtering, and the coefficient of yield is 90.4% (by the amount of adiethylene glycol). And preserve and backup the products. |

鐵桿木蟲 (知名作家)
帝國空軍中將

木蟲 (正式寫手)
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