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【答案】应助回帖
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chunling0102: 金币+6, 博学EPI+1 2013-04-03 20:28:57
参考文献：Patent：SUBSTITUTED THIAZOLE DERIVATIVES BEARING 3-PYRIDYL GROUPS, PROCESS FOR PREPARING THE SAME AND USE THEREOF （ EP1348706 A1, 2003）可在google patent上下载
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). |
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