以均三甲苯为原料,经溴甲基化反应、氧化反应、缩合反应、脱氢氧化反应合成了含能固化剂2,4,6-三甲基间苯二腈氧化物,总收率42%;利用红外光谱、1 H NMR、13C NMR及元素分析等方法对目标化合物和中间体的结构进行了表征;利用DSC分析了2,4...以均三甲苯为原料,经溴甲基化反应、氧化反应、缩合反应、脱氢氧化反应合成了含能固化剂2,4,6-三甲基间苯二腈氧化物,总收率42%;利用红外光谱、1 H NMR、13C NMR及元素分析等方法对目标化合物和中间体的结构进行了表征;利用DSC分析了2,4,6-三甲基间苯二腈氧化物的热分解性能;探讨了溴甲基化和氧化反应的机理,确定了合成2,4,6-三甲基间苯二腈氧化物的最佳工艺条件。结果表明,当氧化反应时间为3d,缩合反应的催化剂为NaOH,脱氢氧化反应NaClO摩尔量为43mmol时,合成的2,4,6-三甲基间苯二腈氧化物产率最高,为73%;2,4,6-三甲基间苯二腈氧化物的腈氧基团相对比较稳定,100℃才开始分解,在室温下即可固化液体聚丁二烯橡胶。展开更多
Grignard reagents were prepared from the starting materials 1-bromo-3,5-difluorobenzene,1-bromo-2,4-difluorobenzene andbromo-3,4-difluorobenzene respectively,then reacted with diethyl carbonate to form magnesium tris(...Grignard reagents were prepared from the starting materials 1-bromo-3,5-difluorobenzene,1-bromo-2,4-difluorobenzene andbromo-3,4-difluorobenzene respectively,then reacted with diethyl carbonate to form magnesium tris(difluoropheny)methanol,and methacryloyl chloride was added dropwise to abtain tris(difluorophenyl)methyl methacrylates.The target products were synthesized in high overall yield(67～74%)with"one-pot"method.Structures of the compounds were comfirmed by IR,1HNMR,13CNMR and elemental analysis,and methanolysis was also studied.展开更多
文摘以均三甲苯为原料,经溴甲基化反应、氧化反应、缩合反应、脱氢氧化反应合成了含能固化剂2,4,6-三甲基间苯二腈氧化物,总收率42%;利用红外光谱、1 H NMR、13C NMR及元素分析等方法对目标化合物和中间体的结构进行了表征;利用DSC分析了2,4,6-三甲基间苯二腈氧化物的热分解性能;探讨了溴甲基化和氧化反应的机理,确定了合成2,4,6-三甲基间苯二腈氧化物的最佳工艺条件。结果表明,当氧化反应时间为3d,缩合反应的催化剂为NaOH,脱氢氧化反应NaClO摩尔量为43mmol时,合成的2,4,6-三甲基间苯二腈氧化物产率最高,为73%;2,4,6-三甲基间苯二腈氧化物的腈氧基团相对比较稳定,100℃才开始分解,在室温下即可固化液体聚丁二烯橡胶。
文摘Grignard reagents were prepared from the starting materials 1-bromo-3,5-difluorobenzene,1-bromo-2,4-difluorobenzene andbromo-3,4-difluorobenzene respectively,then reacted with diethyl carbonate to form magnesium tris(difluoropheny)methanol,and methacryloyl chloride was added dropwise to abtain tris(difluorophenyl)methyl methacrylates.The target products were synthesized in high overall yield(67～74%)with"one-pot"method.Structures of the compounds were comfirmed by IR,1HNMR,13CNMR and elemental analysis,and methanolysis was also studied.
