在线等 帮我翻译一下这段短文 化工专业英语 请不要用软件翻译 谢谢 30

CatalyticreactionswerecarriedoutunderaN2atmosphereusingpre-driedglassware.ortho-Alkyn... Catalytic reactions were carried out under a N2 atmosphere using pre-dried glassware. ortho-Alkynylbromoarenes 1, and 14 were prepared in analogy to previously described methodologies. Other starting materials were obtained from
commercial sources, and were used without further purification.Yields refer to isolated compounds, estimated to be>95% pure as determined by 1H NMR and GC. Flash chromatography:Macherey–Nagel silica gel 60 (70–230 mesh).NMR spectra were recorded on Bruker AMX 600, Varian VXR400S, Bruker AM 250, Unity 300 or Inova 500 instruments in the solvent indicated; chemical shifts (d) are given in ppm.
To a solution of CuI (18 mg, 0.10 mmol, 10 mol%) and KOt-Bu (336 mg, 3.0 mmol) in PhMe (3 mL) was added 1c(265 mg, 1.0 mmol) and 4-methylaniline (129 mg, 1.2 mmol)at ambient temperature. The resulting mixture was stirred at 105 8C for 2 h. CH2Cl2 (50 mL) and aqueous HCl (2N,50 mL) were added to the reaction mixture at ambient temperature.The separated aqueous phase was extracted with CH2Cl2 (250 mL). The combined organic layers were dried over MgSO4 and concentrated under vacuum. The remaining residue was purified by column chromatography on
silica gel (n-pentane/Et2O, 200/1!50/1) to afford 3d as a yellow oil
A suspension of CuI (19 mg, 0.10 mmol, 10 mol%), K2CO3(0.276 g, 2.00 mmol), 4b (0.141 g, 1.20 mmol), 12 (0.026 g,0.30 mmol, 30 mol%) and 1e (0.257 g, 1.00 mmol) in PhMe(4 mL) was stirred under N2 for 24 h at 105 8C. H2O (50 mL)and Et2O (50 mL) were added to the reaction mixture at ambient temperature. The separated aqueous phase was extracted with Et2O (250 mL). The combined organic layers
were dried over MgSO4 and concentrated under vacuum.The remaining residue was purified by column chromatography on silica gel (n-pentane/Et2O 50:1) to afford 5e as a white solid;
Preliminary studies revealed that KO-t-Bu was superior among a variety of bases (e.g., NaO-t-Bu, or LiO-t-Bu). Contrary to palladium-catalyzed transformations, the use of chlorides as leaving groups in substrates 1a and1b, unfortunately, only gave rise to unsatisfactory results
(entries 1, and 2). However, synthetically useful isolated yields were accomplished with ortho-alkynylbromoarenes (entries 3–11). Notably, ortho-substituents on more sterically hindered aniline derivatives were well tolerated (entries 7, and 8), as were chlorides as functionalities, which resulted in the chemoselective preparation of substituted indoles 3i–3k (entries9–11). As to the mechanism of this “nitrogen
ligand-free” copper-catalyzed transformation, experiments with a secondary amine suggest a reaction sequence consisting of intermolecular hydroamination,followed by intramolecular N-arylation.
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aurore1221
2012-01-26
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氮气使用预干燥玻璃器皿的气氛下进行催化反应。比喻先前所描述的方法制备邻Alkynylbromoarenes 1,和14。其他起始原料取自
商业来源,并没有进一步purification.Yields指分离化合物,估计纯度> 95%,经1H NMR和GC确定。闪存色谱仪:马歇雷-内格尔硅胶60(70-230目)核磁共振光谱布鲁克的AMX 600,VXR400S瓦里安,布鲁克AM 250,统一300或500在溶剂中表示INOVA文书记录;化学位移(D)以ppm。
崔(18毫克,0.10毫摩尔,10 mol%的)和噶卜在PhMe(336毫克,3.0毫摩尔)(3毫升)加1C(265毫克,1.0毫摩尔)和4 - 甲基苯胺(129毫克的解决方案,1.2 mmol)的环境温度。由此产生的混合搅拌2小时在105 8C二氯甲烷(50毫升)和水盐酸(2N,50毫升),在环境温度下反应混合物中分离水相提取二氯甲烷(2 50毫升)。合并有机层以上硫酸镁干燥,并集中在真空状态下。剩下的残余物经柱层析
硅胶(n-pentane/Et2O,200 / 1 50 / 1)为黄色油3D负担
一个暂停崔(19毫克,0.10毫摩尔,10 mol%的),碳酸钾(0.276克,2.00毫摩尔),4B(0.141克,1.20毫摩尔),12(0.026克,0.30毫摩尔,30摩尔%)和1E(0.257 G,1.00 mmol)的PhMe(4毫升),搅拌下N2在105℃下24小时。添加到反应混合物在室温下的水(50毫升)和乙醚(50毫升)。水相分离提取乙醚(2 50毫升)。合并有机层
纯化硅胶柱色谱法(n-pentane/Et2O 50:1),干燥硫酸镁下vacuum.The剩余残渣集中负担5E作为一种白色固体。
初步研究表明,KO - T卜基地之间的一个品种(例如,NAO - T卜,或LIO - T - BU)的优越。钯催化转换相反,留在基板1A and1b组使用氯化物,不幸的是,只产生了令人满意的结果
(条目1和2)。然而,综合有用的隔离产量完成与邻alkynylbromoarenes(3-11项)。值得注意的是,更多的空间位阻的苯胺衍生物邻取代,良好的耐受性(条目7和8),以及作为功能的氯化物,导致在化学选择性制备取代吲哚3I - 3K(entries9 11)。至于这个“氮机制
与二级胺配体的铜催化改造,实验表明反应序列的分子hydroamination组成,分子内的N -芳基化反应
心边九益量坑的7216
2012-01-07 · TA获得超过5.8万个赞
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催化反应进行了氮气气氛下使用预干燥的玻璃器皿。ortho-alkynylbromoarenes1,和14准备类似于先前描述的方法。其他原料取自

商业来源,并用于进一步纯化。产量是指化合物,估计“95%纯所确定的核磁共振,气相色谱法。闪光色谱法:使用–格尔硅胶60(70–230目)。核磁共振谱录在布鲁克阿莫西林600,瓦里安vxr400s,布鲁克是250,统一300或诺瓦仪器在500个溶剂表明;化学位移(四)中给出的百万分之一。

一个解崔(18毫克,0.10浓度,10摩尔%)和kot-bu(336毫克,3浓度)在phme(3毫升)增加集成电路(265毫克,1浓度)和4 -甲基苯胺(129毫克,1.2浓度)在环境温度。由此产生的混合物搅拌105笼2小时二氯甲烷(50毫升)和盐酸溶液(2,50毫升)被添加到反应混合物在室温下。分离水相提取与二氯甲烷(250毫升)。合并后的有机层是干超过硫酸镁和集中在真空。剩余的残渣纯化柱层析

硅胶(正戊烷/et2o,200 /1!50 /1)提供三维为黄色油

暂停崔(19毫克,0.10浓度,10摩尔%),碳酸钾(0.276克,2浓度),红(0.141克,1.20浓度),12(0.026克,0.30浓度,30摩尔%)和E(0.257克,1浓度)在phme(4毫升)搅拌下氮气为24小时,105控制。水(50毫升)和et2o(50毫升)被添加到反应混合物在室温下。分离水相提取et2o(250毫升)。合并后的有机层

干燥硫酸镁和集中在真空下。剩余的残渣纯化柱层析硅胶(正戊烷/et2o50 : 1)提供5为白色固体;
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龙飞凤舞吉祥春7842
2012-01-08 · TA获得超过6.5万个赞
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Come and look at my home~The answer is in my room.(小一级英语水平。。。单纯手打~吼吼)

参考资料: In my Da Nao..........

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匿名用户
2012-01-08
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vbshdvh十大好处就萨博cashhas词霸vgvsvdxsv说的不算大慈iasuhchh1,瞎编的,别当真

参考资料: 0.0

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