2—取代苯胺基—3—叔丁基苯并吡嗪的合成

２－取代苯胺基－３－叔丁基苯并吡嗪的合成方东吉成荣（江苏盐城师专科技部盐城２２４００２）关键词２－取代苯胺基－３－叔丁基苯并吡嗪α－（叔丁基）羰基硫代甲酰芳胺中图分类号Ｏ６２６．４１６α－羰基硫代酰胺能与二元胺类化合物反应生成杂环化合物［１］。本文报...     

N-芳基-5-芳基-2-呋喃甲酰胺和N-5-芳基-2-呋喃甲酰基-N′-芳氧基乙酰基肼的合成及生物活性的研究

５－芳基－２－呋喃甲酸及其衍生物具有调节植物生长等作用［４］．我们通过大量的实验，选用ＰＴＣ法，利用５－芳基－２－呋喃甲酰氯与芳胺和芳氧基乙酰肼反应，合成了新化合物Ⅱ和Ⅳ：ＲＣＯＣｌＯ（Ⅰ）ＡｒＮＨ２／ＰＥＧ－４００→ＲＣＯＮＨＡｒ（Ⅱ）ＯＮａＯＨ／...     

N—甲基—N—芳基—2—（4‘—硝基苯硫基）乙酰胺类化合物的合成

先由芳胺合成N-甲基芳胺,再由氯乙酰氯酰化后与对硝基硫酚在相转移催化条件下反应,生成2-(4＇-硝基苯硫基)乙酰芳胺.该法具有操作简便,产率高的优点.     

香草醛—N—酰腙类化合物的合成与表征

Ｓｃｈｉｆｆ碱类化合物和酰腙类化合物大多具有除草,杀菌等生物活性,已有一些报道［１,２］,对该类化合物的深入研究是当今农药界热点之一,表明此类化合物具有广阔的开发前景。据文献报道［１］,香草醛与芳胺反应生成的Ｓｃｈｉｆｆ碱类化合物具有优异的促进植物生根性。为寻求新的具有生物活性的物质,我们采用香草醛与酰肼反应,合成了３种未见报道的酰腙类化合物。其结构经ＩＲ,１ＨＮＭＲ和元素分析证实。合成反应如下：３—ＣＨ３Ｏ—４—ＨＯＣ６Ｈ３ＣＨＯ＋Ｈ２ＮＮＨＣＯ—Ｒ３—ＣＨ３Ｏ—４—ＨＯＣ６Ｈ３ＣＨＮＮＨＣＯ…     

2—芳酰氨基—5—[1—苯基—2—羟基—2—（对甲氧基苯）乙基]—1,3,4—噻二唑的合成

２－芳酰氨基－５－苄基－１，３，４－噻二唑１上５－位苄基在ＥｔＯＮａ／ＥｔＯＨ中生成负离子，再与对甲氧基苯甲醛亲核加成合成了一系列新的２－芳酰氨基－５－［１－苯基－２－羟基－２－（对甲氧基苯）乙基］－１，３，４－噻二唑２．化合物２的结构经元素分析，ＩＲ，＾１Ｈ ＮＭＲ和ＭＳ分析确证，初步观察了２抗菌活性。     

1－苯氧乙酰基－4－芳酰基氨基硫脲的合成

１－苯氧乙酰基－４－芳酰基氨基硫脲的合成贾学顺，王玉炉，王昀（河南师范大学化学系，新乡４５３００２）许多酰氨基硫脲类衍生物具有抗病毒￣［１］、。抗细菌￣［２］、抗肿瘤￣［３］等功效，因而引起人们的广泛注意。为了深入研究此类化合物的性质，作者将具有生物...     

胺桥杯［4］芳烃固相微萃取探头的特性及其应用

采用溶胶-凝胶方法制备了25,27-二羟基-26,28-(1′,10′-二氧代-4′,7′-二氮杂-3′,8′-二氧代亚辛基)-对-特丁基-杯［4］芳烃/羟基硅油(胺桥杯［4］/OH-TSO)固相微萃取(SPME)探头,通过对脂肪胺和芳胺的分析研究了它的特性。该探头具有耐高温、抗溶剂冲洗、使用寿命长、重现性好等特点。杯环上极性胺桥的引入增强了涂层的极性,因而在不需衍生的情况下对脂肪胺和芳胺都具有很好的萃取能力,表现出对胺类化合物的特殊选择性。脂肪胺的检出限为0.19～39.51 μg/L,线性范围达3个数     

芳香硝基物CO选择还原—环境友好芳胺合成新路线

含有羰基、氯、氰基和双键的芳胺类化合物是染料、颜料、医药和农药等领域的重要中间体［1］.然而,它们难以从相应的芳香硝基物与金属氢化物试剂的催化加氢直接制得,因为在这些还原条件下,羰基、氯、氰基和双键也能发生还原反应［2］ .目前,工业上通常还只能用经典的铁粉还原法或硫化碱还原法生产这些芳胺衍生物,但用铁粉还原法,产生的大量铁泥严重污染环境;硫化碱还原法,则存在合成路线复杂、成本高、收率低和废液量大等不足之处［3］ .近年来,一种以CO为还原剂还原芳香硝基物的反应,以其对硝基的高选择性而日益引起人们的兴趣,因而有望成为合成含有羰基、氯和氰基的芳香胺类衍生物的一条环境友好新途径［4］.     

2-(5-芳氧基-4-苯基-1,2,4-三唑-3-硫基)乙酰芳胺的水相合成、 晶体结构及生物活性

在无催化剂存在下, 以水为溶剂通过5-芳氧基-4-苯基-1,2,4-三唑-3-硫酮与氯乙酰芳胺的硫烷基化反应, 合成了14个未见文献报道的2-(5-芳氧基-4-苯基-1,2,4-三唑-3-硫基)乙酰芳胺. 其结构经元素分析, IR和1H NMR进行了表征, 利用单晶X射线衍射法测定了化合物5n的单晶结构. 该化合物通过分子间氢键自组装成三维网状结构的超分子. 生物活性试验表明部分化合物对小麦的根有促进作用而对所有的茎都有抑制活性.     

2-（5-芳氧甲基-4-苯基-1，2,4-三唑-3-硫基）乙酰芳胺的水相合成、晶体结构及生物活性

在无催化剂存在下,以水为溶剂通过5-芳氧甲基-4-苯基-1,2,4-三唑-3-硫酮与氯乙酰芳胺的硫烷基化反应,合成了14个未见文献报道的2-(5-芳氧甲基-4-苯基-1,2,4-三唑-3-硫基)乙酰芳胺.其结构经元素分析,IR和1HNMR进行了表征,利用单晶X射线衍射法测定了化合物5n的单晶结构.该化合物通过分子间氢键自组装成三维网状结构的超分子.生物活性试验表明部分化合物对小麦的根有促进作用而对所有的茎都有抑制活性.     

Sc2MgGa2 and Y2MgGa2

Scandium magnesium gallide, Sc₂MgGa₂, and yttrium magnesium gallide, Y₂MgGa₂, were synthesized from the corresponding elements by heating under an argon atmosphere in an induction furnace. These intermetallic compounds crystallize in the tetragonal Mo₂FeB₂‐type structure. All three crystallographically unique atoms occupy special positions and the site symmetries of (Sc/Y, Ga) and Mg are m2m and 4/m, respectively. The coordinations around Sc/Y, Mg and Ga are pentagonal (Sc/Y), tetragonal (Mg) and triangular (Ga) prisms, with four (Mg) or three (Ga) additional capping atoms leading to the coordination numbers [10], [8+4] and [6+3], respectively. The crystal structure of Sc₂MgGa₂ was determined from single‐crystal diffraction intensities and the isostructural Y₂MgGa₂ was identified from powder diffraction data.     

Zur Kenntnis der Dialkalimetalldichalkogenide β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 und Rb2Te2

On Dialkali Metal Dichalcogenides β-Na₂S₂, K₂S₂, α-Rb₂S₂, β-Rb₂S₂, K₂Se₂, Rb₂Se₂, α-K₂Te₂, β-K₂Te₂ and Rb₂Te₂ The first presentation of pure samples of α- and β-Rb₂S₂, α- and β-K₂Te₂, and Rb₂Te₂ is described. Using single crystals of K₂S₂ and K₂Se₂, received by ammonothermal synthesis, the structure of the Na₂O₂ type and by using single crystals of β-Na₂S₂ and β-K₂Te₂ the Li₂O₂ type structure will be refined. By combined investigations with temperature-dependent Guinier-, neutron diffraction-, thermal analysis, and Raman-spectroscopy the nature of the monotropic phase transition from the Na₂O₂ type to the Li₂O₂ type will be explained by means of the examples α-/β-Na₂S₂ and α-/β-K₂Te₂. A further case of dimorphic condition as well as the monotropic phase transition of α- and β-Rb₂S₂ is presented. The existing areas of the structure fields of the dialkali metal dichalcogenides are limited by the model of the polar covalence.     

Crystal Structures of [Bu2Sn(O2PPh2)2], [Ph2Sn(O2PPh2)2], and [PhClSn(O2PPh2)OMe]2. Raman Spectra of [Ph2Sn(O2PPh2)2] and [PhClSn(O2PPh2)OMe]2

[(n‐Bu)₂Sn(O₂PPh₂)₂] ( 1 ), and [Ph₂Sn(O₂PPh₂)₂] ( 2 ) have been synthesized by the reactions of R₂SnCl₂ (R=n‐Bu, Ph) with HO₂PPh₂ in Methanol. From the reaction of Ph₂SnCl₂ with diphenylphosphinic acid a third product [PhClSn(O₂PPh₂)OMe]₂ ( 3 ) could be isolated. X‐ray diffraction studies show 1 to crystallize in the monoclinic space group P2₁/c with a = 1303.7(1) pm, b = 2286.9(2) pm, c = 1063.1(1) pm, β = 94.383(6)°, and Z = 4. 2 crystallizes triclinic in the space group , the cell parameters being a = 1293.2(2) pm, b = 1478.5(4) pm, c = 1507.2(3) pm, α = 98.86(3)°, β = 109.63(2)°, γ = 114.88(2)°, and Z = 2. Both compounds form arrays of eight‐membered rings (SnOPO)₂ linked at the tin atoms to form chains of infinite length. The dimer 3 consists of a like ring, in which the tin atoms are bridged by methoxo groups. It crystallizes triclinic in space group with a = 946.4(1) pm, b = 963.7(1) pm, c = 1174.2(1) pm, α = 82.495(6)°, β = 66.451(6)°, γ = 74.922(6)°, and Z = 1 for the dimer. The Raman spectra of 2 and 3 are given and discussed.     

Electrochemical study of (NEt4)2Cl2FeS2MoS2 and (NEt4)2Cl2FeS2MoS2FeCl2

Summary The ability of [MoS₄]^2–, anions to be used as ligands for transition metal ions has been widely demonstrated, especially with Fe²⁺. The present study has been restricted to linear complexes such as (NEt₄)₂ [Cl₂FeS₂MoS₂] and (NEt₄)₂[Cl₂FeS₂MoS₂FeCl₂]. Their electrochemical properties are described: upon electrochemical reduction, these compounds yield MoS₂, as a black precipitate, and an iron complex in solution, assumed to be [SFeCl₂]^2–. The electrochemical reduction goes through two electron transfers, coupled with the breakdown of the molecular skeleton: a DISPl and an ECE mechanism. Depending on the solvent, the following equilibrium may be observed: [Cl₄Fe₂MoS₄]^2–[Cl₂FeMoS₄]^2–+FeCl₂. The equilibrium constant, K_D, was evaluated by differential pulse polarography. K_D is tightly related to the donor number of the solvent.     

The alkali hypophosphites KH2PO2, RbH2PO2 and CsH2PO2

The structures of the hypophosphites KH₂PO₂ (potassium hypophosphite), RbH₂PO₂ (rubidium hypophosphite) and CsH₂PO₂ (caesium hypophosphite) have been determined by single‐crystal X‐ray diffraction. The structures consist of layers of alkali cations and hypophosphite anions, with the latter bridging four cations within the same layer. The Rb and Cs hypophosphites are isomorphous.     

Syntheses,Spectroscopic Studies,and Crystal Structures of Me2Sn(O2PPh2)2, Ph2Pb(O2PMe2)2, and Ph2Pb(O2PPh2)2

Me₂Sn(O₂PPh₂)₂ ( 1 ), Ph₂Pb(O₂PMe₂)₂ ( 2 ), and Ph₂Pb(O₂PPh₂)₂ ( 3 ) have been synthesized by the reactions of Me₂SnCl₂ or Ph₃PbCl with the corresponding diorganophosphinic acid in methanol. X‐ray diffraction studies show that the diorganophosphinate groups behave as double bridges between the metal atoms leading to polymeric ring‐chain structures with M₂O₄P₂ (M = Pb, Sn) eight‐membered rings. The organic groups bonded to the metal atoms are in trans‐position in the resulting octahedral arrangement around the metal atoms. The IR and the mass spectra were reported and discussed.     

Thermal decomposition of Me3SnO2PCl2, Me2Sn(O2PCl2)2 and Ph3SnO2PCl2

TG and DTA studies on Me₃SnO₂PCl₂, Me₂Sn(O₂PCl₂)₂ and Ph₃SnO₂PCl₂ were carried out under dynamic argon atmosphere. The results show that the decomposition proceeds in different stages leading to the formation of Sn₃(PO₄)₂ as a stable product. This compound was characterized by IR spectroscopy. Decomposition schemes involving reductive elimination reactions were proposed.