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AnnF版主 (文壇精英)
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[求助]
求助翻譯一段英文，灰常謝謝！��！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
銀蟲 (小有名氣)
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3樓2013-01-02 17:44:49
huang172026
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【答案】應助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
AnnF: 金幣+10, 翻譯EPI+1, ★有幫助, 還得改改，不過還是謝謝了哈 2013-01-02 23:19:51
sltmac: 金幣+40, 歡迎常來本版交流 2013-02-25 09:37:16
AnnF: 金幣+10, 翻譯EPI+1, ★有幫助, 還得改改，不過還是謝謝了哈 2013-01-02 23:19:51
sltmac: 金幣+40, 歡迎常來本版交流 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鹽(HBTU,3.80g, 0.01mol,1.00eq.) 加入裝有磁力攪拌子的烘干圓底燒瓶中，圓底燒瓶通氬氣保護，加橡膠塞或隔膜。然后加入無水二氯甲烷(50 mL) . 攪拌3 min后, 依次加入無水DIPEA (2.58g, 0.02mol,2.0eq.)和芐胺 (0.011 mol, 1.10 eq.) ,反應混合物于室溫攪拌2-4h。反應過程中反應液由稍渾濁變?yōu)榫啵砻鱄BTU已轉(zhuǎn)化完. TLC 跟蹤反應(展開劑: 4% MeOH/CH2Cl2, V/V)。反應液傾入有1N HCl(50 mL)的分液漏斗1 N HCl (50 mL)，二氯甲烷萃取，有機層以1N HCl 洗滌(3×40 mL)，無水硫酸鈉干燥，過濾，真空濃縮。得到淡黃色油狀物轉(zhuǎn)入100-mL燒瓶再溶于二氯甲烷 (40 mL)。一次加入三氟乙酸(10 mL)。攪拌2-4 h，緩慢萃取出二氯甲烷層，冷卻，加入飽和碳酸鈉溶液 (50 mL)，水相以二氯甲烷萃取(3×40 mL)，合并有機層，無水硫酸鈉干燥，過濾，真空濃縮。粗產(chǎn)物以硅膠薄層層析色譜(TLC) 純化(展開劑: 4% MeOH/CH2Cl2, V/V) ，得到中間體Ia-c . 結(jié)構(gòu)由1H NMR、13CNMR、IR、和元素分析(見SI)確認。 |
2樓2013-01-02 17:28:16
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