N,N′-二(芳磺酰)亚磺酰胺-S-(2-苯并咪唑基)类化合物的合成

本文报道了新化合物N,N＇—二(芳磺酰)亚磺酰胺—S—(2—苯并咪唑基)钠(a～e)以及N,N＇—二(芳磺酰)亚磺酰胺—S—(2—苯并咪唑基)(f～i)的合成。通过在感光乳剂中的应用,我们发现a,b和c具有超增感作用,它们分别使卤化银乳剂的感光度提高62％,22％和45％。 钠—N—氯芳磺酰亚胺化合物既是一类精细化工产品,又是一类重要的反应中间体。由它们     

N,N,N',N'-四丁基丙二酰胺从硝酸盐介质中萃取铈(Ⅲ)

核燃料后处理的一个目标是利用中子放射将半衰期很长的锕系元素转变为半衰期短的同位素.由于镧系元素能有效地吸收中子,从而阻止可嬗变的锕系元素捕获中子,所以必须利用溶剂萃取的方法将高放废液中三价的锕系元素与三价的镧系元素分离开来.     

4-芳氧乙(丙)酰氨基苯磺酰胺的合成与除草活性

芳氧羧酸;4-芳氧乙(丙)酰氨基苯磺酰胺的合成与除草活性     

N'-(5-芳基-1,3,4(口恶)二唑-2-基)-N-(邻苯磺酰甲酰亚胺乙酰基)硫脲的合成及抑菌活性

将邻苯甲酰磺酰亚胺、1.3,4-(口恶)二唑2个杂环同时引入到酰基硫脲中,合成了12种新的N'-(5-芳基-1,3,4.(口恶)二唑-2-基)-N-(邻苯磺酰甲酰亚胺乙酰基)硫脲化合物,化合物的结构均经元素分析、1H NMR和IR 等测试技术得以确证.抑菌法生物活性测试结果表明,大部分化合物对黄瓜灰霉病菌、油菜菌核病菌抑制效果很好,特别是化合物5b和5l对5种病菌抑制率均在87%以上,有的病菌抑制率达到100%.     

N,N'-二(糖基硫代亚脲基)芳基硫代膦酰二胺的合成

N;N'-二(糖基硫代亚脲基)芳基硫代膦酰二胺的合成;糖基异硫氰酸酯;硫代膦酰二肼;生物活性     

N,N,N'',N''-四丁基丁二酰胺萃取Tb(Ⅲ)的研究

国内外在四取代双酰胺类萃取剂萃取铀(IV)、钍(IV)的性能研究方面已经做了大量工作[1-3],但对核废料中共存稀土元素的萃取研究较少[4].本文合成了N,N,N',N'-四丁基丁二酰胺(TBSA),详细研究了其萃取Tb(Ⅲ)的性能.     

N,N,N',N'-四丁基丙二酰胺萃取硝酸铥(Ⅲ)

N;N;N';N'-四丁基丙二酰胺萃取硝酸铥(Ⅲ)     

N,N,N',N'-四丁基丙二酰胺萃取铀(VI)的机理

研究了Ｎ,Ｎ,Ｎ’,Ｎ’－四丁基丙二酰胺（ＴＢＭＡ）以甲苯为稀释剂,从硝酸介质中萃取硝酸和铀（Ⅵ）的机理。在该萃取体系中,ＴＢＭＡ和 ＨＮＯ_３形成 ＴＢＭＡ· ＨＮＯ_３,和 Ｕ（Ⅵ）形成为 ＵＯ_２（ＮＯ_３）_２· ３ＴＮＭＡ。借助红外光谱分析,确定了在萃合物中ＮＯ_３~－不参与ＵＯ_２~（２＋）的直接配位,并对萃合物中配体的配位方式进行了讨论。     

N,N-二(2-苯并咪唑亚甲基)甲胺高氯酸盐的晶体和电子结构

合成了三齿配体N,N-二(2-苯并咪唑亚甲基)甲胺(MN3)的高氯酸盐.对该化合物进行了元素分析、紫外和红外表征;采用X射线衍射方法测定了该化合物的晶体结构,依据晶体结构数据使用G98程序对配体(MN3)进行了量子化学计算.     

1,4,7,10-N,N,N,N.四(2-(4-(2-乙酰硫基乙氧基)苯氧基)乙基)-1,4,7,10-四氮杂环十二烷的合成研究

以对苄氧基苯酚为原料,经3步反应合成不对称的对苯二酚烷氧基化合物,并以此为原料,合成乙酰硫基修饰的cyclen四取代氢醌醚链化合物.该路线不仅反应条件温和,操作易行,且收率高,克服了文献报道的合成路线重复性差、收率低的缺点.关键中间体及目标化合物经~1H NMR、~(13)C NMR、MS、IR和元素分析表征.     

2-烷基-2-(芳磺酰基)乙酸酯的高效共轭加成

本文报道在固-液相转移催化的温和条件下2-烷基-2-(芳磺酰基)乙酸酯(1)与α, β-不饱和酯、腈、酮(2)的高选择性和高效率共轭加成反应。成功地合成了2, 2-二取代戊二酸二酯(3a~d)、4-氰基丁酸酯(3e~g)和5-氧代己酸酯(3h~j)。对它们的结构作了表征。初步讨论了本合成法的特点。Michael受体、相转移催化剂和溶剂等对共轭加成反应的影响。     

N,N-二(2-羟乙基)-2-氨基乙磺酸钠的合成研究

采用二乙醇胺与2-氯乙基磺酸钠反应合成N,N-二(2-羟乙基)-2-氨基乙磺酸钠(BES钠盐),由核磁氢谱(1H NMR)和碳谱(13C NMR)、红外光谱(FT-IR)、X射线衍射(XRD)等仪器表征了合成产物的结构和特性.根据反应体系pH值的变化及核磁谱图,确定了BES钠盐的最佳合成工艺:反应物料比为1:1:1,反...     

Synthesis of N,N,N-Triethyl-2-[4-(2-phenylethenyl) phenoxy] ethanammonium iodide

The synthesis of N,N,N-triethyl-2-[4-(2-phenylethenyl) phenoxy] ethanammonium iodide, antispasmodic disubstituted olefin, was achieved via palladium-catalyzed cross-coupling of phenylacetylide with aryl bromide followed by hydroalumination.     

Synthesis of 1-(arylsulfonyl)pyrrolidines from phenols and 1-[(4-chlorophenyl)sulfonyl]-2-ethoxypyrrolidine

Acid-catalyzed reaction of 1-[(4-chlorophenyl)sulfonyl]-2-ethoxypyrrolidine with phenols leads to the formation of new 1-(arylsulfonyl)pyrrolidines. The reaction proceeds under mild conditions and may be used as a convenient method for the synthesis of pyrrolidine-1-sulfonylarene derivatives containing a phenol fragment in the position 2.     

Synthesis and color of 2-(N,N-diethyl-p-quinonediimine)-indazolones

A number of substituted 2-(N, N-diethyl-p-quinonediimine)indazolones have been synthesized, and their optical properties investigated. It has been shown that introduction of electrophilic substituents into the benzene ring of an indazolone gives rise to a bathochromic shift in the absorption spectra of 2-(N, N-diethyl-p-quinonediimine)indazolones in alcohol and benzene solution.     

Synthesis of 2-(2-methoxyethyl)- and 2-(2-thiomethoxyethyl)-aniline and related compounds

Summary 2-(2-Nitrophenyl)-ethanol (2) was methylated with dimethyl sulfate to give 2-(2-methoxyethyl)-1-nitrobenzene (3a) which then was reduced with hydrazine hydrate in the presence ofRaney nickel to 2-(2-methoxyethyl)-aniline (1a). Compound1a can be transformed into the N-monosilylated derivative4 by lithiation withn-butyllithium and subsequent reaction with chlorotrimethylsilane. Reaction of2 withp-toluenesulfonyl chloride yields 2-(2-nitrophenyl)-ethylp-toluenesulfonate (5), which reacts with sodium thiomethoxide to give 2-(2-nitrophenyl)-ethylp-toluenesulfonate (5), which reacts with sodium thiomethoxide to give 2-(2-thiomethoxyethyl)-1-nitrobenzene (3b).3b was reduced with hydrazine hydrate in the presence ofRaney nickel to yield 2-(2-thiomethoxyethyl)-aniline (1b). Ethyl (2-nitrophenyl)-acetate (6) could be dimethylated with methyl iodide in the presence of potassiumtert-butoxide and 18-crown-6 to give ethyl 2-methyl-2-(2-nitrophenyl)-propionate (7). Reduction of7 with lithium borohydride yields 2,3-dihydro-3,3-dimethyl-1H-indole (9) and 2-[(1-hydroxy-2-methyl)-2-propyl]-aniline (10).

---

Synthese von 2-(2-Methoxyethyl)- und 2-(2-Thiomethoxyethyl)-anilin und verwandten Verbindungen

Zusammenfassung 2-(2-Nitrophenyl)-ethanol (2) wurde mit Dimethylsulfat zu 2-(2-Methoxyethyl)-1-nitrobenzol (3a) methyliert, das sich mit Hydrazinhydrat in Gegenwart vonRaney-Nickel zu 2-(2-Methoxyethyl)-anilin (1a) reduzieren läßt. Verbindung1a kann durch Metallierung mitn-Butyllithium und anschließende Reaktion mit Chlortrimethylsilan in dasN-monosilylierte Derivat4 umgewandelt werden. Reaktion von2 mitp-Toluolsulfonylchlorid ergab 2-(2-Nitrophenyl)-ethyl-p-Toluolsulfonat (5), das mit Natriumthiomethanolat zu 1-Nitro-2-(2-thiomethoxyethyl)-benzol (3b) reagiert.3b wurde mit Hydrazinhydrat in Gegenwart vonRaney-Nickel zu 2-(2-Thiomethoxyethyl)-anilin (1b) reduziert. Ethyl-2-(nitrophenyl)-acetat (6) kann mit Methyliodid in Gegenwart von Kalium-tert-butoxid und 18-Krone-6 zu Ethyl-2-methyl-2-(2-nitrophenyl)-propionat (7) dimethyliert werden. Reduktion von7 mit Lithiumborhydrid lieferte 2,3-Dihydro-3,3-dimethyl-1H-indol (9) und 2-[(1-Hydroxy-2-methyl)-2-propyl]-anilin (10).

     

New phosphorescent polynuclear Cu(I) compounds based on linear and star-shaped 2-(2'-pyridyl)benzimidazolyl derivatives: syntheses, structures, luminescence, and electroluminescence

Four dinuclear and trinuclear Cu(I) complexes that contain 2-(2'-pyridyl)benzimidazolyl derivative ligands including 1,4-bis[2-(2'-pyridyl)benzimidazolyl]benzene (1,4-bmb), 1,3-bis[2-(2'-pyridyl)benzimidazolyl]benzene (1,3-bmb), 1,3,5-tris[2-(2'-pyridyl)benzimidazolyl]benzene (tmb), and 4,4'-bis[2-(2'-pyridyl)benzimidazolyl]biphenyl (bmbp) have been synthesized. The formulas of these complexes are [Cu(2)(1,4-bmb)(PPh(3))(4)][BF(4)](2) (1), [Cu(2)(1,3-bmb)(PPh(3))(4)][BF(4)](2) (2), [Cu(3)(tmb)(PPh(3))(6)][BF(4)](3) (3), and [Cu(2)(bmbp)(PPh(3))(4)][BF(4)](2) (4), respectively. The crystal structures of 2-4 have been determined by single-crystal X-ray diffraction analyses. The Cu(I) ions in the complexes have a distorted tetrahedral geometry. For 3, two structural isomers (syn and anti) resulted from two different orientations of the three 2-(2'-pyridyl)benzimidazolyl chelating units were observed in the crystal lattice. Variable-temperature (1)H NMR experiments established the presence of syn and anti isomers for 1-3 in solution which interconvert at ambient temperature. Complexes 1-4 have a weak MLCT absorption band in the 350-450 nm region and display a yellow-orange emission when irradiated by UV light. One unexpected finding is that the yellow-orange emission of complexes 1-4 has a very long decay lifetime (approximately 200 micros) at 77 K. An electroluminescent (EL) device using 4 as the emitter and PVK as the host was fabricated. However, the long decay lifetime of the copper complexes may limit their applications as phosphorescent emitters in EL devices.     

新型2-甲基-6-(N,N-二烷基氨基)喹喔啉的合成

以4-硝基邻苯二胺为原料，经缩合、硝基还原和N-烷基化反应合成了一系列具有新颖结构的2-甲基-6-(N,N-二烷基氨基)喹喔啉，其结构经¹H NMR, ¹³C NMR, HR-MS（ESI）和XRD表征。