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AnnF版主 (文坛精英)
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[求助]
求助翻译一段英文，灰常谢谢！！！急！！！
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Phenylalanine (2.65 g, 0.01 mol, 1.0 0 equiv.) and O-benzotriazol-1-yl-N,N,N,N-tetramethyl- uronium hexafl uorophosphate (HBTU,3.80g, 0.01mol,1.00equiv.) were loaded into an oven-dried round-bottomed flask equipped with a magnetic stir bar, rubber septum, and argon inlet. Anhydrous dichloromethane (50 mL) was then added. Af ter 3 min, anhydrous DIPEA (2.58g, 0.02mol,2.0equiv)and benzylamine (0.011 mol, 1.10 equiv.) were sequentially added and the reaction mixture was stirred at room temperature for2-4h. During the process, the state of the solution was seen to change from slightly heterogeneous to homogeneous con firming the consumption of HBTU. And the reaction was followed by TLC (developing solvent: 4% MeOH/CH2Cl2, V/V). The reaction mixture was poured into a separatory funnel containing 1 N HCl (50 mL), and was then partitioned between dichloromethane and aqueous hydrochloric acid solution. The organic layer was washed with 1N HCl (3×40 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo . The resulting light yellow oil was transferred to a 100-mL flask and redissolved in dichloromethane (40 mL).Trifl uoroacetic acid (10 mL) was then added in one portion. After 2-4 h, the mixture was slowly partitioned with dichloromethane and chilled, saturated aqueous sodium carbonate solution (50 mL)was added. The aqueous layer was extracted with dichloromethane(3×40 mL), and the combined organic extracts were dried over anhydrous sodium sulfate,fi ltered, and concentrated in vacuo . The crude product was puri fi ed by thin layer chromatography (TLC) on a silica gel (developing solvent: 4% MeOH/CH2Cl2, V/V) to give theintermediates Ia ec . The structure was con fi rmed by1H NMR,13CNMR, IR, and elemental analysis (see the Supporting Information).  原文2.jpg [ Last edited by AnnF on 2013-1-2 at 16:19 ] |
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huang172026
银虫 (小有名气)
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3楼2013-01-02 17:44:49
huang172026
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【答案】应助回帖
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AnnF: 金币+10, 翻译EPI+1, ★有帮助, 还得改改，不过还是谢谢了哈 2013-01-02 23:19:51
sltmac: 金币+40, 欢迎常来本版交流 2013-02-25 09:37:16
AnnF: 金币+10, 翻译EPI+1, ★有帮助, 还得改改，不过还是谢谢了哈 2013-01-02 23:19:51
sltmac: 金币+40, 欢迎常来本版交流 2013-02-25 09:37:16
| 苯丙氨酸(2.65 g, 0.01 mol, 1.0 0 eq.)和O-(1H-苯并三唑-1-基)-N,N,N',N'-四甲基硫尿六氟磷酸盐(HBTU,3.80g, 0.01mol,1.00eq.) 加入装有磁力搅拌子的烘干圆底烧瓶中，圆底烧瓶通氩气保护，加橡胶塞或隔膜。然后加入无水二氯甲烷(50 mL) . 搅拌3 min后, 依次加入无水DIPEA (2.58g, 0.02mol,2.0eq.)和苄胺 (0.011 mol, 1.10 eq.) ,反应混合物于室温搅拌2-4h。反应过程中反应液由稍浑浊变为均相，表明HBTU已转化完. TLC 跟踪反应(展开剂: 4% MeOH/CH2Cl2, V/V)。反应液倾入有1N HCl(50 mL)的分液漏斗1 N HCl (50 mL)，二氯甲烷萃取，有机层以1N HCl 洗涤(3×40 mL)，无水硫酸钠干燥，过滤，真空浓缩。得到淡黄色油状物转入100-mL烧瓶再溶于二氯甲烷 (40 mL)。一次加入三氟乙酸(10 mL)。搅拌2-4 h，缓慢萃取出二氯甲烷层，冷却，加入饱和碳酸钠溶液 (50 mL)，水相以二氯甲烷萃取(3×40 mL)，合并有机层，无水硫酸钠干燥，过滤，真空浓缩。粗产物以硅胶薄层层析色谱(TLC) 纯化(展开剂: 4% MeOH/CH2Cl2, V/V) ，得到中间体Ia-c . 结构由1H NMR、13CNMR、IR、和元素分析(见SI)确认。 |
2楼2013-01-02 17:28:16
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