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[求助]
求翻译一段化学反应资料（英译汉）
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说明：此段英文里面有些部分看得不是很明白，希望高手能够准确将英文的意思翻译过来，因为之前按自己理解的意思做反应效果不是很好，自己英文水平不高，想确认下是不是理解错啦，物料部分可以不用翻译，谢谢 To a stirred suspension of sodium hydride (60% dispersion in mineral oil, 6.28 g, 157 mmol) in N,Ndimethylformamide(150 mL) under nitrogen at 0 ° C. was added portion wise N-(2-hydroxyethyl)phthalimide (2, 20 g, 105 mmol). The reaction mixture was then allowed to warm to ambient temperature with stirring for 30 minutes. To a stirred suspension in a separate flask of sodium hydride (60% dispersion in mineral oil, 6.28 g, 157 mmol) in N,N-dimethylformamide (150 mL) under nitrogen at 0 ° C. was added portion wise methyl 4-chloroacetoacetate (1,12.1 ml, 105 mmol). The reaction mixture was then allowed to warm to ambient temperature with stirring for 30 minutes. The two reaction mixtures were then combined portion wise and stirred at ambient temperature under nitrogen for 6 hours. After cooling to 0 ° C., a further portion of sodium hydride (2.0 g, 50.0 mmol) was added. The mixture was stirred for 10 minutes at 0° C., then a further portion of methyl 4-chloroacetoacetate (3.0 ml, 26.0 mmol) was added. The reaction mixture was then stirred at ambient temperature for 18 hours, then poured onto a mixture of ice and saturated ammonium chloride, and then neutralized with aqueous HCl (10 N). The precipitate which formed was filtered off and recrystallized from ethyl acetate to give a first crop of 3 as a yellow solid. The combined filtrates were extracted with ethyl acetate (3x300 mL). The combined organic layers were washed with saturated brine (2x300 mL) and water (300 mL), dried over MgSO4 and concentrated under reduced pressure to leave a residue which was purified by column chromatography over silica gel (50 g pre-packed Isolute® column) using ethyl acetate/hexane (1:1) as eluent to give a second crop of 3 as a yellow solid, which was combined with the first crop to give methyl 4-((2'- hydroxyethyl)phthalimide)acetoacetate, yield 10.8 g, 34% |
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wangy32188: 金币+40, 翻译EPI+1, ★★★很有帮助, 20 2013-01-07 18:00:52
wangy32188: 金币+40, 翻译EPI+1, ★★★很有帮助, 20 2013-01-07 18:00:52
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氮气保护下，钠氢溶于N，N-二甲基甲酰胺中，降温至0度，分批加入N-（2 - 羟乙基）邻苯二甲酰亚胺。加料完毕，升至室温，搅拌30min. 氮气保护下，于另一烧瓶中，钠氢溶于N，N-二甲基甲酰胺中，降温至0度，分批加入4 - 氯乙酰乙酸甲酯。加料完毕，升至室温，搅拌30min. 两个反应采用双滴加（或者双双分批加入，视具体情况而定），于室温氮气保护下搅拌6h.冷却至0度，再加NaH一批。混合液于0度搅拌10min，再加一批4 - 氯乙酰乙酸甲酯。混合液室温下搅拌18h,倒入饱和氯化氨和冰的混合液中，HCl进行中和。得到的沉淀抽滤，经EA结晶得到第一批产品3，黄色固体。滤液经EA萃取3次，合并有机层，依次经过饱和食盐水（2次）和水洗涤。MgSO4干燥，浓缩。得到的残留物经过硅胶柱分离(洗脱剂为EA:Hex = 1:1)，得到第二批产品3.两批合并，得到methyl 4-((2'- hydroxyethyl)phthalimide)acetoacetate 10.8g,产率34%。 注意：根据楼主提供的资料，这个反应是严格的无水无氧反应，在加料的过程中还要采用分批次来进行，特别是双滴加，如果是悬浮液，最好分批，否则难以操作，并可能会产生副产物。楼主操作时要当心，实验中最好采用TLC和HPLC进行检测。 以上是本人的理解，如有不当，请帮忙指正，谢谢！ |
5楼2012-12-30 10:45:15