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请高手翻译一段话，不要机器翻译 A. 2-(3,4-Dimethoxyphenyl)-N,N-dimethylacetamidine . An oven-dried, 250-mL, single-necked, round-bottomed flask containing a 3-cm magnetic stirring bar is charged with 7.96 g (0.045 mol) of (3,4-dimethoxyphenyl)acetonitrile (Note 1) and 4.95 g (0.050 mol) of copper(I) chloride (Note 2), fitted with a septum, flushed with argon, and maintained under a static pressure of argon using a gas bubbler. Using a 20-mL gas-tight syringe, 45 mL (0.067 mol) of a 1.5 M ethanolic solution of dimethylamine (Note 3) is added successively in three 15-mL portions at room temperature with vigorous stirring. The heterogeneous pale brown mixture is then heated at 70°C for 24 hr, during which time it becomes brown-red. The mixture is cooled to room temperature and poured with vigorous stirring into a 250-mL Erlenmeyer flask containing 70 mL of aqueous 30% sodium hydroxide and 100 mL of diethyl ether (Note 4); the mixture was stirred vigorously for 3 min. The organic layer is separated, and the aqueous layer is extracted with three 75-mL portions of diethyl ether (Note 5). The combined organic extracts are dried over sodium sulfate and filtered through a sintered glass funnel layered with 2 cm of Celite. The solid residue is washed with diethyl ether (20 mL). The combined filtrate and washings are concentrated by rotary evaporation followed by drying under reduced pressure (0.1 mm) for 1.5 hr to provide 9.1-9.4 g (93-96% yield) of a dark brown oil (Note 6),(Note 7). The compound is stored under argon at −18°C until used in step B. |
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liumingchang
铁杆木虫 (正式写手)
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2楼2009-11-10 15:46:52
3楼2009-11-10 21:55:45
4楼2009-11-11 18:49:58
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昨晚化了1-2个小时已经搞定了，因此放弃求助，全文如下： A, 2-(3,4-二甲氧基苯基)-N,N-二甲基乙脒 在烘干的250mL圆底单口烧瓶中放入一只3cm长的搅拌磁子、7.96g(0.045mol)3,4-二甲氧基苯乙腈(注释1)和4.95g(0.050mol)氯化亚铜(注释2)，装上隔膜，用氩气吹赶后，用鼓泡器保持体系氩气的静态压力。在室温与快速搅拌下,使用20mL的气密注射器，将45mL1.5mol/L(0.067mol)的二甲胺乙醇溶液(注释3)分3次连续地加入(每次加15mL)。然后使非均相的浅棕色反应混合物在70℃恒温反应为24h，随着反应的进行，反应混合物的颜色逐渐变成棕红色。反应毕，将反应液冷却至室温，边快速搅拌边将反应液慢慢倒入盛有70mL30%的氢氧化钠水溶液和100mL乙醚(注释4)的250mL锥形烧瓶中，所得混合物继续搅拌3min后静置分层，分去有机层，水层用乙醚萃取3次(每次用乙醚75mL(注释5))。合并有机相，无水硫酸钠干燥后，用铺有2cm厚的硅藻土的烧结玻璃漏斗过滤，滤饼用20mL乙醚洗涤。合并滤液和洗涤液，旋蒸除去溶剂乙醚，残留物在减压(0.1 mm)下干燥1.5h,得咖啡色油状物9.1-9.4 g(产率93-96%)(注释6) (注释7)。所得化合物在进行B步骤之前应于−18℃，氩气氛围保存。 |
5楼2009-11-11 18:52:03