采用2-氯-4-碘-5-三氟代甲基吡啶为起始原料,与正丁基锂溶液反应制备5-三氟甲基-2-氯-4-吡啶硼酸。实验研究了合成反应过程几种反应条件对合成产率的影响情况,采用HPLC,FTIR,1 H NMR等方法对产品的纯度和结构进行了分析表征。实验结果表...采用2-氯-4-碘-5-三氟代甲基吡啶为起始原料,与正丁基锂溶液反应制备5-三氟甲基-2-氯-4-吡啶硼酸。实验研究了合成反应过程几种反应条件对合成产率的影响情况,采用HPLC,FTIR,1 H NMR等方法对产品的纯度和结构进行了分析表征。实验结果表明:当反应温度为-70℃,反应时间为2h,反应物料配比n(2-氯-4-碘-5-三氟代甲基吡啶)∶n(硼酸三丁酯)∶n(正丁基锂)为1.00∶1.20∶1.20,溶液pH值为9.0时,5-三氟甲基-2-氯-4-吡啶硼酸的收率为83.10%,纯度可达98.65%以上。展开更多
Pyridin-a-ylmethyl 3,5-bis(pyridin-a-ylmethoxy)benzoate(a=2,L1;a=3,L2;a=4,L3)were synthesized by reaction of 3,5-dihydroxybenzoic acid and a-chloromethyl pyridine(a=2,3,4).Their structures were characterized by IR,1H ...Pyridin-a-ylmethyl 3,5-bis(pyridin-a-ylmethoxy)benzoate(a=2,L1;a=3,L2;a=4,L3)were synthesized by reaction of 3,5-dihydroxybenzoic acid and a-chloromethyl pyridine(a=2,3,4).Their structures were characterized by IR,1H NMR,13C NMR,ESI-MS and elemental analysis.The effects of reaction temperature and reaction time on esterification and etherification were also studied,respectively.展开更多
文摘采用2-氯-4-碘-5-三氟代甲基吡啶为起始原料,与正丁基锂溶液反应制备5-三氟甲基-2-氯-4-吡啶硼酸。实验研究了合成反应过程几种反应条件对合成产率的影响情况,采用HPLC,FTIR,1 H NMR等方法对产品的纯度和结构进行了分析表征。实验结果表明:当反应温度为-70℃,反应时间为2h,反应物料配比n(2-氯-4-碘-5-三氟代甲基吡啶)∶n(硼酸三丁酯)∶n(正丁基锂)为1.00∶1.20∶1.20,溶液pH值为9.0时,5-三氟甲基-2-氯-4-吡啶硼酸的收率为83.10%,纯度可达98.65%以上。
文摘Pyridin-a-ylmethyl 3,5-bis(pyridin-a-ylmethoxy)benzoate(a=2,L1;a=3,L2;a=4,L3)were synthesized by reaction of 3,5-dihydroxybenzoic acid and a-chloromethyl pyridine(a=2,3,4).Their structures were characterized by IR,1H NMR,13C NMR,ESI-MS and elemental analysis.The effects of reaction temperature and reaction time on esterification and etherification were also studied,respectively.
