4-Methylbenzaldehyde and 2-methylbenzaldehyde are oxidated by iodine in the mixture of THF and ammonia water at room temperature to give p-tolunitrile and o-tolunitrile in 87.1% and 82.0% yield respectively.p-Tolunitrile is nitrated with fuming nitric acid in concentrated sulfuric acid below 0℃ to produce 4-methyl-3-nitrobenzonitrile in 88.4% yield,and for o-tolunitrile to afford 2-methyl-5-nitrobenzonitrile in 79.6% yield.Their structures are characterized by IR and 1H NMR spectra respectively.
UO2(EPC)2(EPC=5-ethyl-3-pyridinecarboxylate)was synthesized by the hydrothermal reaction of UO2(NO3)2 ·6H2O with imazethapyr [2-(4,5-dihydro-4-methyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl)-5-ethyl-3-pyridine-carboxylic acid] at 120 ℃,which 2-(4,5-dihydro-4-methyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl group was removed under this condition to result in the formation of 5-ethyl-3-pyridinecarboxylate ligand(EPC).The structure and fluorescent property of the synthesized complex is also reported.CCDC:645641.
研究了季铵盐型阳离子改性淀粉絮凝剂的微波辐射合成.该工艺反应时间短、产率高、操作简便,同时有效抑制了副反应的发生,提高了产品纯度.讨论了诸因素对反应的影响,通过正交试验确定了反应的最佳条件为:氢氧化钠、2,3-环氧丙基三甲基氯化铵与淀粉的摩尔比1.4∶1∶2.2,辐射反应时间1.5 m in,微波功率280 W.