銀催化的酰胺與N-甲基吡咯烷酮的sp~3C-N官能化反應(yīng)
發(fā)布時間:2018-04-28 14:37
本文選題:C-N鍵 + 交叉偶聯(lián)反應(yīng); 參考:《甘肅農(nóng)業(yè)大學(xué)學(xué)報》2016年06期
【摘要】:【目的】研究交叉脫氫偶聯(lián)(cross-dehydrogenative-coupling,CDC)反應(yīng)機(jī)理及條件,尋求一種新的合成方法,最終實現(xiàn)酰胺與N-甲基吡咯烷酮sp3 C-N官能化反應(yīng).【方法】根據(jù)酰胺與N-甲基吡咯烷酮sp~3C-N官能化反應(yīng)的反應(yīng)機(jī)理和反應(yīng)路徑,對該反應(yīng)可能的催化劑AgNO_3,FeCl_3,CuCl_2,CuCl,NiSO_4·6H_2O,Fe_2(SO_4)_3·xH_2O,SnCl_2·2H_2O,CuI,BiCl_3,CoCl_2·6H_2O及氧化劑TBHP,Ca(ClO)_2,K2S_2O_8等化合物進(jìn)行了篩選,同時優(yōu)化了反應(yīng)條件.【結(jié)果】最佳催化劑為AgNO_3,氧化劑為K_2S_2O_8,最佳反應(yīng)條件為溫度75℃,反應(yīng)時間4h,溶劑為體積分?jǐn)?shù)50%的乙腈水溶液.合成了6種不同的酰胺衍生物,它們的產(chǎn)率在64%~75%之間.用核磁1 H譜和紅外光譜鑒定合成新化合物的結(jié)構(gòu),表明這些化合物都是酰胺與N-甲基吡咯烷酮反應(yīng)的主產(chǎn)物.【結(jié)論】該方法是一種實現(xiàn)交叉脫氫偶聯(lián)(cross-dehydrogenative-coupling,CDC)反應(yīng)的高效綠色的合成方法.
[Abstract]:[objective] to study the mechanism and conditions of cross-dehydrogenative coupling (CDCC) reaction, and to find a new synthesis method. Finally, the functionalization of amide with N-methylpyrrolidone sp3 C-N was realized. [methods] according to the reaction mechanism and path of sp~3C-N functionalization between amide and N-methylpyrrolidone, The possible catalysts for this reaction, AgNOSP, FeCl _ 3, CuCl _ 3, CuCl _ 2, CuCl _ 2 / Niso _ 4 H _ 2O _ 2 / C _ 2H _ 2O _ 2 / C _ 2H _ 2O _ 4 & S _ 2S _ 2O _ 4, were screened, and the reaction conditions were optimized. [results] the best catalyst is Agno _ 3, the oxidizer is K _ 2S _ 2O _ 8, the optimum reaction condition is 75 鈩,
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