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chunling0102銀蟲 (小有名氣)
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[求助]
3-醛基-4-溴吡啶或3-醛基-4-氯吡啶的合成
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| 有哪位大哥大姐做過3-醛基-4-溴吡啶或3-醛基-4-氯吡啶, 原料用4-溴吡啶或4-氯吡啶鹽酸鹽。我想要具體的操作過程和后處理過程,及收率 |
金蟲 (正式寫手)
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參考文獻(xiàn):Patent:SUBSTITUTED THIAZOLE DERIVATIVES BEARING 3-PYRIDYL GROUPS, PROCESS FOR PREPARING THE SAME AND USE THEREOF ( EP1348706 A1, 2003)可在google patent上下載 A solution (50 ml) of 4-chloropyridine (25.0 g, 0.22 mol) in tetrahydrofuran was added dropwise to a tetrahydrofuran solution (300 ml) of lithium diisopropylamide prepared from a solution (179 ml, 0.29 mol) of 1.6 M n-butyllithium in hexane and diisopropylamine (33.4 g, 0.33 mol) under an argon atmosphere at -78 DEG C. After stirring for 30 min., DMF (19.3 g, 0.26 mol) was added and the mixture was gradually heated to room temperature. The reaction mixture was extracted with ethyl acetate (200 ml) - 5percent NH4Cl aq. (300 ml). The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure to give a crude title compound (27 g, 86percent) as an oil.<1>H-NMR (200Hz, CDCl3) delta : 7.45 (1H, d, J = 5.0 Hz), 8.69 (1H, d, J = 5.0Hz), 9.05 (1H, s), 10.51 (1H, S). |
金蟲 (正式寫手)
| https://www.google.com.hk/patent ... NG+3-PYRIDYL+GROUPS,+PROCESS+FOR+PREPARING+THE+SAME+AND+USE+THEREOF&hl=zh-CN&sa=X&ei=dWlaUcqGFoPhlAW694DIAg&ved=0CEIQ6AEwAw |
木蟲之王 (文學(xué)泰斗)
聯(lián)合國小木蟲水區(qū)資深代言人
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木蟲之王 (文學(xué)泰斗)
聯(lián)合國小木蟲水區(qū)資深代言人
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