三苄基锡(IV)炔基(烯基)膦酸衍生物的合成及结构表征

Six novel tribenzyltin(IV) dervatives of alkynyl or alkenyl Phosphonic acid (PhCH₂)₃SnOP(O)(OH)R, Where R=C≡CPh, C≡CC₃H₇ n,C≡CC₄H₉ n, C≡CC₅H₁₁ n,C≡CC₆H₁₃ n, CH=CClPh,were synthesized by resaction of the monosodium salt of the alkynyl or alkenyl phosphonic acid with tribenzyltin(IV) chloride in benzene. Their structures were cheracterized by elementary analysis, IR,¹H NMR, ¹¹⁹Sn NMR, MS and TG DTA. The results showed that these compounds arefive coordinated -O-P-O-bridged polymers.     

α,ω-二(1-H-苯并三唑基)烷烃的合成和生物活性的研究

在相转移催化剂存在下,以苯并三唑为原料与二卤代烷反应合成了4个新的α,ω-二(1-H-苯并三唑基)烷烃,它们的结构经元素分析,IR和1H NMR证实.初步考查了它们的生物活性.     

微波辐射下双(2-苯并咪唑基)烷烃的合成

微波辐射条件下合成了7种双（2－苯并咪唑基）烷烃,为这类化合物的合成提供了一种新方法,相比于常规反应,反应时间大为缩短且产率相当。     

2-(2,4-二氟苯基)-1-(4-烃基派嗪-1-基)-3-(1,2,4-三唑-1-基)-2-丙醇类化合物的合成及抗真菌活性

近20年来,真菌感染特别是深部真菌感染日益引起人们的广泛关注[1]。三唑类抗真菌药物对真菌的选择性较高,代谢稳定,体内动态、安全性都较好,已成为目前抗真菌药物研究开发的重点[2]。三唑类抗真菌药物是细胞色素P450 14α 去甲基酶的抑制剂,可影响该酶所催化的真菌麦角甾醇的生物合成,导致真菌细胞膜破损而死亡[3,4]。1998年,SynPhar实验室及Taiho制药公司[5]研制开发的化合物Syn 2869采用了取代哌嗪作为侧链。体外实验表明,该化合物抗菌谱广,对多种念珠菌、隐球菌及曲莓菌均有效,体内实验中,与目前临床上治疗真菌感染的主要用药伊曲…     

2,3,3,3-四氟丙烯的合成研究

本文综述了目前2,3,3,3-四氟丙烯（HFO-1234yf）的合成路线,包括氟-氯交换、脱卤化氢、脱卤、脱卤醇、脱次氯酸乙酰酯、脱水、加氢脱卤、脱氢、高温热解、SF₄参与的氟化反应、脱羧等。其中,以2-氯-3,3,3-三氟丙烯（HCFO-1233xf）为原料的氟-氯交换路线、以1,1,1,2,3-五氟丙烷（HFC-245eb）为原料的脱氟化氢路线和2-氯-1,1,1,2-四氟丙烷（HCFC-244bb）为原料的脱氯化氢路线均具有原料容易合成得到、容易实现气相连续化大规模生产的优势,具有工业化价值。另外,分析对这些路线拥有独立知识产权的氟化工企业现状,提出今后HFO-1234yf领域的研究重点。     

微波辐射无溶剂条件下快速合成2,4,6-三芳基吡啶四氟硼酸盐

在微波辐射无溶剂条件下快速、高产率地合成了2,4,6-三芳基吡啶四氟硼酸盐化合物, 并对其进行核磁共振、红外光谱、元素分析表征. 同时得到了化合物4f的晶体, 对其进行了X单晶射线衍射表征. 结果表明, 该晶体属正交晶系, 空间群Pbca, a＝2.1050(2) nm, b＝1.64360(17) nm, c＝2.9209(3) nm, α＝β＝90.00°, γ＝90.00°, D_c＝1.276 g•cm^－3, V＝10.1057(17) nm^－3, Z＝16.     

两个含双(3,5－二甲吡唑基)甲烷配体的铅(II)配合物的合成与结构表征

Reactions of lead（Ⅱ） nitrate or perchlorate with bis（3,5-dimethylpyrazolyl）methane （dmpzm）, produced two new Pb（Ⅱ） chelated complexes [Pb（dmpzm）2X2] （X=NO3^- 1, ClO4^- 2）. Both compounds were structurally characterized by elemental analysis, IR spectroscopy, thermal analysis, and single crystal X-ray diffraction. Both compounds are mononuclear with a distorted square antiprismatic PbN4O4 coordination geometry incorporating a pair of O,O＇-bidentate anions and N,N＇-bidentate dmpzm ligands. In the crystals of 1 or 2, the methyl or methylene groups of dmpzm ligand interact with the oxygen atoms of nitrates or perchlorates to afford intra- and intermolecular hydrogen bonding, thereby forming a two-dimensional network 1 or a three-dimensional structure 2.     

银配合物[Ag(OPOQ)](BF4)(OPOQ=O,O′-双(8-喹啉基)-1,3二氧丙烷)的合成与表征

四氟硼酸银和配体O,O′-双(8-喹啉基)-1,3-二氧丙烷(OPOQ)反应,生成标题配合物[Ag(OPOQ)](BF4) (C21H18AgBF4N2O2 , Mr = 525.05 ), 并通过了元素分析、红外光谱、核磁氢谱及X-单晶结构表征.配合物的晶体为单斜晶系,空间群为P21/n, 晶胞参数a = 12.009(6), b = 14.594(7), c = 12.124(6)(A); β= 111.875(8)(, V = 1972.0(17)(A)3,Dc = 1.769 g/cm3, Z = 4, ((MoKα) = 1.081 mm-1, F (000) = 1048, S = 1.066.最终偏离因子R = 0.0336, wR = 0.0414.晶体结构显示,该配合物的阳离子是一个半包围的弓形结构.     

3，6-双（3’-氨基呋咱-4-基）-1，4-二氧杂-2，5-二氮杂环己-2，5-二烯的合成及晶体结构

以3-氨基-4-酰胺肟基呋咱（AAOF）为原料合成出了含能化合物3-氨基-4-酰氯肟基呋咱（ACOF）。用稀碱3％～5％Na2CO3水溶液处理，ACOF脱去一分子HCl生成不稳定中间体3-氨基-4-氰基呋咱的氧化物（ACFO），随后发生歧化反应，生成3，4-二（氨基呋咱基）氧化呋咱（BAFF）及其异构体3，6-双（3’-氨基呋咱-4-基）-1，4-二氧杂-2，5-二氮杂环己-2，5-二烯（BADDD）。用IR、MS、^1H NMR、^13C NMR和元素分析对ACOF的分子结构进行了表征。分子和晶体结构测试表明，BADDD是一具有新颖化学分子结构的化合物。     

基于5-磺酸基间苯二甲酸钠和双三唑烷烃的Cu(Ⅱ)配合物的合成、结构和性质

利用5-磺酸基间苯二甲酸钠(NaH₂sip)和双三唑烷烃,合成了3个配合物[Cu_0.5(btm)(H₂O)](H₂sip)·H₂O}_n (1,btm=双三唑甲烷),{[Cu(btp)₂(H₂sip)(H₂O)](NO₃)·4H₂O}_n (2,btp=双三唑丙烷) 和{[Cu(btb)₂(Hsip)]_n (3,btb=双三唑丁烷)。化合物1为一维双链结构;化合物2为二维四方网络结构,多个二维层依次叠加形成三维超分子结构;化合物3也具有二维层状结构,其中金属铜离子和双三唑丁烷构成的一维双链结构经双齿μ₂-Hsip^2-配体连接构成了二维层状结构。同时对配合物的热稳定性和顺磁共振特性进行了讨论。     

NaBF4催化合成二吲哚甲烷类化合物

在乙醇水溶液中,以Na BF4为催化剂,通过吲哚与芳香醛间的串联反应合成了二吲哚甲烷衍生物。考察了催化剂种类、反应介质、温度、反应时间等因素对反应的影响,在优化条件下以较高产率得到了一系列目标产物。     

Convenient Synthesis of Bis(indol)alkanes by Niobium(V) Chloride

Bis(indolyl)alkanes have been synthesized in excellent yields in the presence of a catalytic amount of niobium(V) chloride under solvent-free conditions.     

Efficient Synthesis of Bis(4-Dimethaminophenyl)arylmethanes and Bis(4-Diamethaminophenyl)alkanes Using Iodine Reagent

A novel synthetic utility of NaICl₂ for the preparation of bis(4-dimethaminophenyl)arylmethanes and bis(4-dimethaminophenyl)alkanes is described. In the presence of an aqueous solution of NaICl₂, the reaction of arenes with aromatic aldehydes gives corresponding triarylmethane derivatives regioselectively in moderate to good yields. The method is also useful for the preparation of diarylalkane derivatives by using aliphatic aldehydes.

Supplemental materials are available for this article. Go to the publisher's online edition of Synthetic Communications ^® to view the free supplemental file.     

Convenient Synthesis and Anticancer Activity of Bis(aryl)alkanes and Bis(indolyl)methane Alkaloid Analogs

Russian Journal of General Chemistry - An efficient metal free high yield method of synthesis of bis(indolyl)methanes (BIMs) and bis(aryl)alkanes analogs in the presence of B(C6F5)3 by condensation...     

有机磷酸催化合成双吲哚烷烃衍生物

以联萘二酚衍生的有机磷酸为催化剂,催化吲哚和羰基化合物的亲电取代反应,合成了一系列双吲哚衍生物,收率64%～95%,其结构经1H NMR,13C NMR和HR-MS确证。     

Approaches to the Synthesis of Dicarboxylic Derivatives of Bis(pyrazol-1-yl)alkanes

Carboxylation of bis(pyrazol-1-yl)alkanes by oxalyl chloride was studied. It was found that 4,4′-dicarboxylic derivatives of substrates with electron-donating methyl groups and short linkers (from one to three methylene groups) can be prepared using this method. Longer linkers lead to significantly lower product yields, which is probably due to instability of the intermediate acid chlorides that are initially formed in the reaction with oxalyl chloride. Thus, bis(pyrazol-1-yl)methane gave only monocarboxylic derivative even with a large excess of oxalyl chloride and prolonged reaction duration. An alternative approach involves the reaction of ethyl 4-pyrazolecarboxylates with dibromoalkanes in a superbasic medium (potassium hydroxide–dimethyl sulfoxide) and is suitable for the preparation of bis(4-carboxypyrazol-1-yl)alkanes with both short and long linkers independent of substitution in positions 3 and 5 of pyrazole rings. The obtained dicarboxylic acids are interesting as potential building blocks for metal-organic frameworks.     

Cobalt‐Catalyzed Enantioselective Synthesis of Chiral gem‐Bis(boryl)alkanes

We report an asymmetric synthesis of enantioenriched gem‐bis(boryl)alkanes in an enantioselective diborylation of 1,1‐disubstituted alkenes catalyzed by Co(acac)₂/(R)‐DM‐segphos. A range of activated and unactivated alkenes underwent this asymmetric diborylation in the presence of cyclooctene as a hydrogen acceptor, affording the corresponding gem‐bis(boryl)alkanes with high enantioselectivity. The synthetic utility of these chiral organoboronate compounds was demonstrated through several stereospecific derivatizations and the synthesis of sesquiterpene and sesquiterpenoid natural products.     

无溶剂条件下碘催化不对称双吲哚的合成

在室温以及无溶剂条件下,吲哚与烷基-3-吲哚基甲醇在碘的催化下以73％～99％的高收率得到不对称双吲哚烷基化合物。其结构经^1H NMR,IR及MS表征。