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wuxuepeng木虫 (正式写手)
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【求助】求助翻译。。。
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1 Triethylene Glycol Di(toluene-p-sulphonate) In a 250-mL flask containing 100 mL of THF, were added ptoluenesulfonylchloride (42.0 g, 220 mmol) (recrystallized in pentane) and triethylene glycol (11.0 g, 73.2 mmol). A solution of KOH (26.2 g in 25 mL of water, 467 mmol) is added. The addition was performed for 3 h at 0◦C. After this addition, the mixture was allowed to stand to ambient temperature for 7 h. Then the reaction is poured into 150 mL of a mixture of ice/CH2Cl2 (70/30). The water phase was extracted 3 times with 50 mL of CH2Cl2. The organic phases, dried over MgSO4 and evaporated under vacuum, gave 31.3 g (68.3 mmol) of a yellow oil 2 At room temperature, in a 2-L flask, containing sodium terbutoxide (prepared by a 12-h reaction of Na [8.8 g, 383 mmol] in 1.5 L of tBuOH, at 50◦C), were added drop by drop, simultaneously, triethylene glycol di(toluene-p-sulphonate) (32 g, 69.8 mmol) in 100 mL of dioxane and diethanolamine (8.10 g, 77.0 mmol) in 100 mL of tBuOH. After the addition, the reaction was continued for 3 h at 40◦C. Then the reaction mixture was filtered and the solvent was evaporated. Water (80 mL) was added to the residue and the solution was extracted once with hexane to remove hexane-soluble materials and then was extracted several times with dichloromethane. The dichloromethane extracts were combined, the solvent was evapored, and the residue was distilled (kugelrohr) to give a colorless liquid 谢谢各位高手~~~  |
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jw227
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qingfeng877680(金币+8,VIP+0):谢谢您的翻译！呵呵~~ 10-10 19:03
qingfeng877680(金币+8,VIP+0):谢谢您的翻译！呵呵~~ 10-10 19:03
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二（甲苯-对磺酸基）-二缩三乙二醇 在250毫升圆底烧瓶中称取100毫升四氢呋喃，对甲苯磺酰氯（42.0克，220毫摩尔）（戊烷中重结晶）和三甘醇（11.0克，73.2毫摩尔），反应溶剂是氢氧化钾水溶液（26.2克溶于 25毫升的水，467毫摩尔）。加入固体药品后在0摄氏度反应3小时。接着，室温放置7小时。然后，反应液倒入150毫升的 冰/二氯甲烷混合物（70/30）。每次50ml二氯甲烷提取水相，共3 次。有机相用无水硫酸镁干燥，蒸干二氯甲烷，得到 31.3克（68.3毫摩尔）黄色的油状物2。在室温下，在2 L圆底烧瓶加入叔丁醇钠（钠[8.8克，383 mmol]在 1.5升tBuOH中50摄氏度下反应制备），同时，逐滴加入溶于100ml二氧六环的（甲苯-对磺酸基）-二缩三乙二醇 （32克，69.8 mmol） 和 溶于100毫升叔丁醇中的二乙醇胺（8.10克，77.0毫摩尔）。加完后，反应在40摄氏度进行3小时。然后过滤，蒸干溶剂。再加入水（80毫升），正己烷提取一次，丢掉。再用二氯甲烷提取若干次。二氯甲烷提取液合并，蒸干，重蒸得到无色油状液体。 |
2楼2009-09-06 13:27:09
wuxuepeng
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3楼2009-09-06 15:06:36
