A novel organic disulfide, 2,2 diaminophenyloxydisulfide(DAPD) has been prepared by the reaction of o aminophenol with sulfur monochloride in THF. Its polymer films are formed by electropolymerization from a AN/THF ...A novel organic disulfide, 2,2 diaminophenyloxydisulfide(DAPD) has been prepared by the reaction of o aminophenol with sulfur monochloride in THF. Its polymer films are formed by electropolymerization from a AN/THF solution containing 0.1 mol/L LiClO 4, 0.1 mol/L HCl and 0.05 mol/L DAPD monomer on Pt electrode under continuous cycling between -0.30 V and 1.20 V vs . Ag/AgCl (sat. KCl) at scanning rate 50 mV/s. The cyclic voltammetry shows that its electrochemical behavior is similar to that of polyaniline. The redox peak current of the cyclic voltammograms increase with increasing of the cyclic times. The electronic conductivity of poly (DAPD) can reach from 2.1×10 -3 to 8.7×10 -3 S/cm. Two main facts are considered to be necessary for obtaining electroactive poly (DAPD) in electropolymerization process. One is the existence of sufficient concentration of the supporting electrolyte to enhance the ionic conductivity of AN/THF solution and the other is the existence of protons from the acid HCl. With an increase in acid content of the solution, the polymerization efficiency as well as the electroactivity of poly (DAPD) films show a striking enhancement and the electronic conductivity of poly (DAPD) film increases. But the concentration of HCl would be quite high to result in the decomposition of DAPD monomer.展开更多
Three kinds of 4-(4-aminophenoxy)-2-(alkyl carbamoyl)pyridines were synthesized respectively from three kinds of N-alkyl-4-chloro-2-pyridine carboxamides and p-aminophenol potassium,which were obtained from p-aminophe...Three kinds of 4-(4-aminophenoxy)-2-(alkyl carbamoyl)pyridines were synthesized respectively from three kinds of N-alkyl-4-chloro-2-pyridine carboxamides and p-aminophenol potassium,which were obtained from p-aminophenol and tert-butyl alcohol potassium with nitrogen protection in anhydrous DMF.The structures of the target compounds were characterized by IR,1HNMR and ESI-MS.展开更多
2-(3-(4-methoxyphenoxy)propyl)propane-1,3-diethanethioate is synthesized from 4-methoxyphenol and 1,3-dibromopropane after five-step reaction.The overall yield is 21.2%.The key intermediates and the target compound ar...2-(3-(4-methoxyphenoxy)propyl)propane-1,3-diethanethioate is synthesized from 4-methoxyphenol and 1,3-dibromopropane after five-step reaction.The overall yield is 21.2%.The key intermediates and the target compound are analysized by 1HNMR,13CNMR,IR and MS.展开更多
4-(4-氨基苯氧基)-2-(甲基氨甲酰基)吡啶是合成索拉非尼的重要中间体,它可由Williamson反应合成。以离子液体为溶剂,以NaOH、无水K2CO3为碱,N-甲基-(4-氯-2-吡啶基)甲酰胺和对氨基苯酚为原料,通过Williamson反应合成出目标产物。研究了...4-(4-氨基苯氧基)-2-(甲基氨甲酰基)吡啶是合成索拉非尼的重要中间体,它可由Williamson反应合成。以离子液体为溶剂,以NaOH、无水K2CO3为碱,N-甲基-(4-氯-2-吡啶基)甲酰胺和对氨基苯酚为原料,通过Williamson反应合成出目标产物。研究了影响此反应的一些影响因素,如离子液体种类、反应温度、时间、碱等,并在此研究基础上得出了较佳的反应条件为:以[BMIM][BF4]为溶剂,对氨基苯酚与氢氧化钠的摩尔比为1∶1.1,与无水碳酸钾的摩尔比为1∶0.6,反应温度75℃,反应时间4h,在此条件下所得的收率为89%,产品结构由1 H NMR所证实。另外,离子液体至少可循环使用5次,而对收率及纯度无明显影响,有利于环保。展开更多
以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾...以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾向发烟硫酸和2,6-二氨基吡嗪-1-氧化物混合物中加料的工艺路线,总产率为35%。用1 H NMR,IR,MS对DAPO和LLM-105的结构进行了表征,推测了DAPO环化反应历程。展开更多
文摘A novel organic disulfide, 2,2 diaminophenyloxydisulfide(DAPD) has been prepared by the reaction of o aminophenol with sulfur monochloride in THF. Its polymer films are formed by electropolymerization from a AN/THF solution containing 0.1 mol/L LiClO 4, 0.1 mol/L HCl and 0.05 mol/L DAPD monomer on Pt electrode under continuous cycling between -0.30 V and 1.20 V vs . Ag/AgCl (sat. KCl) at scanning rate 50 mV/s. The cyclic voltammetry shows that its electrochemical behavior is similar to that of polyaniline. The redox peak current of the cyclic voltammograms increase with increasing of the cyclic times. The electronic conductivity of poly (DAPD) can reach from 2.1×10 -3 to 8.7×10 -3 S/cm. Two main facts are considered to be necessary for obtaining electroactive poly (DAPD) in electropolymerization process. One is the existence of sufficient concentration of the supporting electrolyte to enhance the ionic conductivity of AN/THF solution and the other is the existence of protons from the acid HCl. With an increase in acid content of the solution, the polymerization efficiency as well as the electroactivity of poly (DAPD) films show a striking enhancement and the electronic conductivity of poly (DAPD) film increases. But the concentration of HCl would be quite high to result in the decomposition of DAPD monomer.
文摘Three kinds of 4-(4-aminophenoxy)-2-(alkyl carbamoyl)pyridines were synthesized respectively from three kinds of N-alkyl-4-chloro-2-pyridine carboxamides and p-aminophenol potassium,which were obtained from p-aminophenol and tert-butyl alcohol potassium with nitrogen protection in anhydrous DMF.The structures of the target compounds were characterized by IR,1HNMR and ESI-MS.
文摘2-(3-(4-methoxyphenoxy)propyl)propane-1,3-diethanethioate is synthesized from 4-methoxyphenol and 1,3-dibromopropane after five-step reaction.The overall yield is 21.2%.The key intermediates and the target compound are analysized by 1HNMR,13CNMR,IR and MS.
文摘4-(4-氨基苯氧基)-2-(甲基氨甲酰基)吡啶是合成索拉非尼的重要中间体,它可由Williamson反应合成。以离子液体为溶剂,以NaOH、无水K2CO3为碱,N-甲基-(4-氯-2-吡啶基)甲酰胺和对氨基苯酚为原料,通过Williamson反应合成出目标产物。研究了影响此反应的一些影响因素,如离子液体种类、反应温度、时间、碱等,并在此研究基础上得出了较佳的反应条件为:以[BMIM][BF4]为溶剂,对氨基苯酚与氢氧化钠的摩尔比为1∶1.1,与无水碳酸钾的摩尔比为1∶0.6,反应温度75℃,反应时间4h,在此条件下所得的收率为89%,产品结构由1 H NMR所证实。另外,离子液体至少可循环使用5次,而对收率及纯度无明显影响,有利于环保。
文摘以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾向发烟硫酸和2,6-二氨基吡嗪-1-氧化物混合物中加料的工艺路线,总产率为35%。用1 H NMR,IR,MS对DAPO和LLM-105的结构进行了表征,推测了DAPO环化反应历程。
