 |
 |
 |
 |
 |
 |
||
 |
 |
 |
 |
 |
| 3 | 1/1 | 返回列表 |
| 查看: 785 | 回復(fù): 2 | |||
| 本帖產(chǎn)生 1 個 翻譯EPI ，點(diǎn)擊這里進(jìn)行查看 | |||
AnnF版主 (文壇精英)
|
[求助]
求助翻譯一段英文，灰常謝謝�。�！急�。�！
|
||
|
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 ] |
回復(fù)此樓» 猜你喜歡
生物學(xué)學(xué)碩，一志愿湖南大學(xué)，初試成績338
已經(jīng)有6人回復(fù)
-
321求調(diào)劑
已經(jīng)有7人回復(fù)
-
343求調(diào)劑
已經(jīng)有4人回復(fù)
-
305求調(diào)劑
已經(jīng)有3人回復(fù)
-
本科新能源科學(xué)與工程，一志愿華理能動285求調(diào)劑
已經(jīng)有6人回復(fù)
-
332求調(diào)劑
已經(jīng)有3人回復(fù)
-
學(xué)碩274求調(diào)劑
已經(jīng)有8人回復(fù)
-
壓國家一區(qū)線，求導(dǎo)師收留，有恩必謝！
已經(jīng)有7人回復(fù)
-
081200-11408-276學(xué)碩求調(diào)劑
已經(jīng)有4人回復(fù)
-
22408 359分調(diào)劑
已經(jīng)有4人回復(fù)
huang172026
銀蟲 (小有名氣)
- 翻譯EPI: 1
- 應(yīng)助: 6 (幼兒園)
- 金幣: 23.6
- 散金: 58
- 紅花: 1
- 帖子: 269
- 在線: 281.8小時
- 蟲號: 918790
- 注冊: 2009-12-02
- 性別: GG
- 專業(yè): 合成藥物化學(xué)
【答案】應(yīng)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(hù)，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(yīng)混合物于室溫攪拌2-4h。反應(yīng)過程中反應(yīng)液由稍渾濁變?yōu)榫�，表明HBTU已轉(zhuǎn)化完. TLC 跟蹤反應(yīng)(展開劑: 4% MeOH/CH2Cl2, V/V)。反應(yīng)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(jī)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(jī)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(rèn)。 |
2樓2013-01-02 17:28:16
huang172026
銀蟲 (小有名氣)
- 翻譯EPI: 1
- 應(yīng)助: 6 (幼兒園)
- 金幣: 23.6
- 散金: 58
- 紅花: 1
- 帖子: 269
- 在線: 281.8小時
- 蟲號: 918790
- 注冊: 2009-12-02
- 性別: GG
- 專業(yè): 合成藥物化學(xué)
3樓2013-01-02 17:44:49
相關(guān)版塊跳轉(zhuǎn)
我要訂閱樓主 AnnF 的主題更新
| 3 | 1/1 | 返回列表 |
| 最具人氣熱帖推薦 [查看全部] | 作者 | 回/看 | 最后發(fā)表 | |
|---|---|---|---|---|
|
[考研] 材料與化工272求調(diào)劑 +9 | 阿斯蒂芬2004 2026-03-28 | 9/450 |
|
|---|---|---|---|---|
|
[考研] 070305高分子化學(xué)與物理 304分求調(diào)劑 +4 | c297914 2026-03-28 | 4/200 |
|
|
|
[考研]
 一志愿廈門大學(xué)化學(xué)學(xué)碩307求調(diào)劑
+10
|
y7czhao 2026-03-26 | 10/500 |
|
|
|
[考研] 材料與化工（0856）304求B區(qū)調(diào)劑 +8 | 邱gl 2026-03-27 | 8/400 |
|
|
|
[考研] 藥學(xué)105500求調(diào)劑 +3 | Ssun。。 2026-03-28 | 3/150 |
|
|
|
[考研] 295求調(diào)劑 +5 | 1428151015 2026-03-27 | 6/300 |
|
|
|
[考研] 0856材料化工調(diào)劑 總分330 +10 | zhubinhao 2026-03-27 | 10/500 |
|
|
|
[考研] 330一志愿中國海洋大學(xué) 化學(xué)工程 085602 有讀博意愿 求調(diào)劑 +3 | wywy.. 2026-03-27 | 4/200 |
|
|
|
[考研] 070300化學(xué)求調(diào)劑 +4 | 起個名咋這么難 2026-03-27 | 4/200 |
|
|
|
[考研] 一志愿吉大071010，316分求調(diào)劑 +3 | xgbiknn 2026-03-27 | 3/150 |
|
|
|
[考研] 求調(diào)劑 +8 | Auroracx 2026-03-22 | 8/400 |
|
|
|
[考研] 網(wǎng)絡(luò)空間安全0839招調(diào)劑 +4 | w320357296 2026-03-25 | 6/300 |
|
|
|
[考研] 求b區(qū)院校調(diào)劑 +4 | 周56 2026-03-24 | 5/250 |
|
|
|
[考研] 289材料與化工（085600）B區(qū)求調(diào)劑 +4 | 這么名字咋樣 2026-03-22 | 5/250 |
|
|
|
[考研] 340求調(diào)劑 +5 | 話梅糖111 2026-03-24 | 5/250 |
|
|
|
[考研] 生物學(xué)學(xué)碩求調(diào)劑 +7 | 小羊睡著了? 2026-03-23 | 10/500 |
|
|
|
[考研] 材料專碩331求調(diào)劑 +4 | 鮮當(dāng)牛 2026-03-24 | 4/200 |
|
|
|
[考研] 333求調(diào)劑 +3 | ALULU4408 2026-03-23 | 3/150 |
|
|
|
[考研] 315分，誠求調(diào)劑，材料與化工085600 +3 | 13756423260 2026-03-22 | 3/150 |
|
|
|
[考研] 求調(diào)劑一志愿海大，0703化學(xué)學(xué)碩304分，有大創(chuàng)項目，四級已過 +6 | 幸運(yùn)哩哩 2026-03-22 | 10/500 |
|