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1.
Reaction between 3,4,5-triamino-1,2,6-thiadiazine 1,1-dioxides and aldehydes, in acetic acid or DMF, under anhydrous conditions, leads to a mixture of imidazo[4,5-c]- and pyrazino[2,3-c]-1,2,6-thiadiazine derivatives. The ratio of both compounds depends on the nature of the aldehydes used. The same reaction, in the absence of solvent, affords, only pyrazinothiadiazine derivatives. The uv, 1H- and 13C-nmr data of the new compounds are reported.  相似文献   

2.
Reactivity towards alkylating agents in relation to the capacity to bind sodium ions of 1,2,6-thiadiazine 1,1-dioxide derivatives is described. The compounds studied are: 1 , 4-nitro-, 2 , 4-cyano-, 3 ,4-ethoxycarbonyl-2H,6H-1,2,6-thiadiazin-3-one 1,1-dioxide and 4 , 3-amino-4-cyano-6H-1,2,6-thiadiazine 1,1-dioxide. Methylation with dimethyl sulfate of 4-nitro- and 4-cyanothiadiazines 1 and 2 , which show the capacity to bind sodium ions, takes place regioselectively at position 2, whilst the thiadiazines which lack this feature ( 3 and 4 ) are methylated at 2 and 6, and 6 respectively. On using diazomethane, in the absence of alkaline ions, no selectivity was observed. Glycosidation reactions of 1, 3 and 4 have also been carried out. The structure of the newly synthesized compounds are discussed on the basis of their analytical and spectroscopic data.  相似文献   

3.
We have synthesized the three Schiff-base ligands H2L1–H2L3 and their CoII, FeIII and RuIII metal complexes. All compounds have been characterized by analytical and spectroscopic methods. Oxidation of cyclohexane has been done by the metal complexes in CH3CN using H2O2 and/or t-butylhydroperoxide (TBHP) as a co-catalyst. The keto-enol tautomeric forms of the ligands have been studied in polar and non-polar organic solvents. Electrochemical properties of the complexes have been studied at different scan rates. Thermal studies were carried out for the compounds. The ligands H2L1–H2L3 were mutagenic on Salmonella Typhimurium TA 98 strain in the presence and/or absence of S9 mix. While the ligands H2L1 and H2L2 showed mutagenic activity on the strain TA 100 with and without S9 mix, the ligand H2L3 was not mutagenic for TA 100. Antimicrobial activity studies of the compounds have also been carried out.  相似文献   

4.
Changes in the absorption and fluorescence spectra of 1,2,2,3-tetramethyl-(1), 1,2,2,4-tetramethyl-(2), 6-ethoxy-1,2,2,4-tetramethyl-(3), and 1,2,6-trimethyl-1,2-dihydroquinolines (4) were studied in aqueous solution over a wide pH range from 1.0 to 12.0. The quantum yields of fluorescence and the values of pK a of dihydroquinolines (DHQs) under study in the ground and excited states were determined, pK a = 4.5, 3.8, 4.5, and 4.2 for the ground state of compounds 1–4, respectively, and pK a ∼ 1.7 for the S 1* state for all DHQs.  相似文献   

5.
3,5-Diaryl-4H-1,2,6-thiadiazin-4-ones react with NaBH4 to give the 3,5-diaryl-4H-1,2,6-thiadiazin-4-ols and with MeLi to give 4-methyl-3,5-diaryl-4H-1,2,6-thiadiazin-4-ols. The latter dehydrate with p-toluenesulfonic acid to give (3,5-diarylthiadiazin-4-ylidene)methanes. (3,5-Diphenyl-4H-1,2,6-thiadiazin-4-ylidene)methane 15 suffers mono bromination with NBS to give bromo(3,5-diphenyl-4H-1,2,6-thiadiazin-4-ylidene)methane 17. Dichloro- and dibromo(3,5-diphenyl-4H-1,2,6-thiadiazin-4-ylidene)methanes 18 and 19 are formed directly from the 3,5-diphenylthiadiazin-4-one 9 via the Appel reaction using Ph3P and CCl4 or CBr4, respectively. 3,5-Diarylthiadiazin-4-ones treated with P2S5 give 3,5-diarylthiadiazine-4-thiones that react with tetracyanoethylene oxide to give the (thiadiazin-4-ylidene)malononitriles. Finally, the 3,5-diphenylthiadiazine-4-thione 20 reacts with ethyl diazoacetate to give ethyl 2-(3,5-diphenyl-4H-1,2,6-thiadiazin-4-ylidene)acetate 26. The above reactions show that a variety of substitutions at C-4 of 3,5-diaryl substituted 1,2,6-thiadiazin-4-ones can be achieved, which extends the potential applications of this heterocycle. All compounds are fully characterized and a brief comparison of their spectroscopic properties is given.  相似文献   

6.
The P3-nortricyclane 4-methyl-1,2,6-triphosphatricyclo[2.2.1.02,6]heptane, CH3C(CH2P)3, (1), is synthesized in a better yield than earlier described from P4, a Na/K alloy, and CH3C(CH2Br)3 in boiling 1,2-dimethoxyethane. It reacts withM(CO)5 thf (M=Cr, W) in the molar ratios of 1:1, 1:2, and 1:3 to form the pentacarbonylmetal complexes CH3C(CH2P)3[M(CO)5] n [n=1, 2, 3;M=Cr (a), W (b)], (2 a, b–4 a, b).1 gives with Mo(CO)5 thf only mixtures of CH3C(CH2P)3[Mo(CO)5] n andcis-Mo(CO)4 derivatives, which were identified by their infrared active A1 v(CO) modes at 2075 and 2025 cm–1.All the new compounds have been characterized also by their1H{31P},31P{1H} NMR, IR,Raman, and mass spectra.
  相似文献   

7.
The new compound C10H6P(S)[NSi(CH3)3]2P(S) ( 3 ) which contains a P2N2 heterocycle has been prepared in low yield by partial thermal decomposition of 1-{[N,N′-bis(trimethylsilyl)acetamidinium]sulfido}-3-(trimethylsilylamino)-1 H,3 H,1 λ5,3 λ5-naphtho[1,8 a,8-cd][1,2,6]thiadiphosphinine-1,3-dithione [CH3C{NHSi(CH3)3}2]+[C10H6P(S)(NHSiMe3)SP(S)2] ( 2 ). Reaction of 2 with potassium hydroxide in acetonitrile gives the completely desilylated product [CH3C(NH2)2]+[C10H6P(S)(NH2)SP(S)2] ( 4 ). The structures of the new compounds 3 and 4 were elucidated by FTIR and NMR spectroscopy methods and by X-ray structure analyses.  相似文献   

8.
Nitro compounds have been actively researched as driven by their potential to be high‐performing energetic materials. Herein, three new nitro compounds including semicarbazide 3,5‐dinitrobenzoate, (SCZ)(DNBA), manganese 3,5‐dinitrobenzoate dihydrate, [Mn(DNBA)2(H2O)2]n, and bis(semicarbazide) manganese(II) 3,5‐dinitrobenzoate, Mn(SCZ)2(DNBA)2, were synthesized and characterized by elemental analysis, IR spectroscopy, and single‐crystal X‐ray diffraction analysis. The results indicated that the above mentioned compounds are ionic, polymeric, and molecular in nature, respectively. Moreover, their thermal decomposition properties were assessed by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Their non‐isothermal reaction kinetics parameters, critical temperature of thermal explosion (Tbp), entropy of activation (ΔS), enthalpy of activation (ΔH), and free energy of activation (ΔG) of the exothermic decomposition process were also calculated. Results suggest that there was a relationship between the structure and thermal stability.  相似文献   

9.
The new, chiral silylphosphite compounds (O,O-dimethyl-L-tartrato)POSiR3, (R3 = Ph3, tBuMe2, Et3) have been synthesised and their activity as asymmetric phosphonylating reagents investigated.  相似文献   

10.
新型席夫碱大环化合物的合成   总被引:5,自引:0,他引:5  
袁泽利  张奇龙  朱必学 《有机化学》2006,26(11):1590-1593
利用Mn2+, Ba2+作为模板离子, 由邻苯二胺和α,ω-二(3'-羟基-4'-甲酰苯氧基)取代烷[即1,4-二(3'-羟基-4'-甲酰苯氧基)丁烷、1,6-二(3'-羟基-4'-甲酰苯氧基)己烷、1,8-二(3'-羟基-4'-甲酰苯氧基)辛烷]反应分别合成了系列新型大环席夫碱化合物Ln (n=4, 6, 8). Mn2+用于L4合成, 并在洗涤时自动解络; L6L8的合成以Ba2+模板, L6L8的Ba2+配合物经与Na2SO4水溶液反应解络, 得到自由大环配体L6L8. 上述新型大环席夫碱化合物采用元素分析, 1H NMR, IR, 紫外-可见光谱和MS等进行组成和结构表征.  相似文献   

11.
Hydrazonecarboxamides and hydrazonecarbothioamides and their derivatives have important pharmacodynamic significance. In the search for better fungicides and bactericides, organoboron(III) compounds derived from these ligands were screened for their antifungal and antibacterial activities. The heterocyclic aldimines were prepared by the condensation of (2-furanyl)methanal, (2-thienyl)methanal, (2-pyridinyl)methanal, (1H-indol-3-yl)methanal or 3-phenyl-2-propenal with hydrazinecarboxamide or hydrazine-carbothioamide. Unimolar and bimolar reactions between phenyldihydroxyborane and these ligands have produced PhB(OH)(NO), PhB(NO)2, PhB(OH)(NS) and PhB(NS)2 types of biologically active compounds. Structural assignment has been made through UV, IR and NMR (1H, 11B and 13C) spectroscopy. TGA and XRD of a representative compounds have also been carried out. The compounds were tested in vitro against a number of fungal and bacterial strains and were found to possess moderate to good toxicity.  相似文献   

12.
The mass spectra of some α-substituted phenyl-α,α′-dimethoxyl ketones (compounds 1) and their 2,4-dinitrophenylhydrazones (compounds 2) and semicarbazones (compounds 3) have been studied. The characteristic fragments at m/z (M ? 73) from compounds 1, m/z (M ? 253) from compounds 2 and m/z (M ? 130) from compounds 3 are abundant and proposed to be [ArCROCH3]+. Fragmentations yielding [M+ ? 49] from compounds 2 are abnormal and probably involve the methoxyl and nitro groups. The intense peak at m/z 130 due to [CH3OCH2CNNHCONH2]+ from compounds 3 corresponds to α-cleavage of the molecular ion. Some other fragments from these new compounds are interpreted in this paper.  相似文献   

13.
o-Benzoylbenzenesulfonyl chlorides (I) were prepared conveniently from aminobenzophenones by diazotization followed by reaction with sulphur dioxide in the presence of Cu+, according to the general method of Meerwein. Reaction of the sulfonyl chlorides with hydrazine led to 4-phenyl-2H-1,2,3-benzothiadiazine-1,1-dioxides (II). The latter compounds could be methylated and acetylated readily in the 2-position. The 2-methyl derivative (III) could be prepared also by reaction of the sulfonyl chloride (Ia) with methylhydrazine. Catalytic hydrogenation of 6-chloro-4-phenyl-2H-1,2,3-benzothiadiazine-1,1-dioxide (IIa) gave the 3,4-dihydro derivative (V). Reaction of the sulfonyl chlorides (I) with o-phenylenediamine followed by cyclodehydration led to 11H-11,11a-dihydrobenzimidazo[1,2-b] [1,2]benzisothiazole-5,5-dioxides (VII). One of the latter compounds (VIIa) in sodium hydroxide solution in the presence of methyl iodide or benzyl chloride was transformed into 6-methyl- and 6-benzyl-5H-dibenzo[c,g] [1,2,6]thiadiazocine-5,5-dioxides (VIII), respectively. 5H-Dibenzo[c,g] [1,2,6] thiadiazocine-6,6-dioxides (XIV) were prepared also by cyclodehydration of 2-amino-2′-benzoylbenzenesulfonanilides (XIII).  相似文献   

14.
Superhalogens, owing to their large electron affinity (EA, exceeding those of any halogen atom), play an essential role in physical chemistry as well as new material design. They have applications in hydrogen storage and lithium-ion batteries. Owing to the unique geometries and electronic features of magnesium-based clusters, their potential to form a new class of lithium salts has been investigated here theoretically. The idea is assessed by conducting ab initio computations on Li+/MgnF2n+1-2mOm compounds (n=2, 3; m=0-3) and analyzing their performance as potential Li-ion battery electrolytes. The Mg3F7 cluster, with large electron binding energy (EA of 7.93 eV), has been proven to serve as a building block for lithium salts. It is shown that, apart from high electronic stability, the new superhalogen-based electrolytes exhibit a set of desirable properties, including a large band gap, high electrolyte stability window, easy mobility of the Li+, and favorable insensitivity to water.  相似文献   

15.
Efficient OLED devices have been fabricated using organometallic complexes of platinum group metals. Still, the high material cost and low stability represent central challenges for their application in commercial display technologies. Based on its innate stability, gold(III) complexes are emerging as promising candidates for high-performance OLEDs. Here, a series of alkynyl-, N-heterocyclic carbene (NHC)- and aryl-gold(III) complexes stabilized by a κ3-(N^C^C) template have been prepared and their photophysical properties have been characterized in detail. These compounds exhibit good photoluminescence quantum efficiency (ηPL) of up to 33 %. The PL emission can be tuned from sky-blue to yellowish green colors by variations on both the ancillary ligands as well as on the pincer template. Further, solution-processable OLED devices based on some of these complexes display remarkable emissive properties (ηCE 46.6 cd.A−1 and ηext 14.0 %), thus showcasing the potential of these motifs for the low-cost fabrication of display and illumination technologies.  相似文献   

16.
Two series of trialkyltin carboxylates containing butyl and cyclohexyl groups on tin, BunCy3-nSnO2CR (n = 1, 2; R = n-Pr, Ph, 4-CIC6H4, 4-NO2C6H4) have been synthesized and their structures characterized by IR, and 119Sn and 13C NMR spectroscopies. The compounds are five-coordinate, carboxylate-bridged polymers when R = n-Pr, while the other aromatic carboxylates are four coordinate. The compounds were also tested for their fungicidal, insecticidal and acaricidal activities.  相似文献   

17.
Cyclocondensations with Primary Sulfinimidamides: Synthesis of Six-membered Rings with λ4-Thiadiazine and λ4-Thiatriazadiphosphorine Constitution 1,1-Dimethyl-ethanesulfinimidamide ( 1 ,) reacts with tetracyanoethylene by elimination of hydrogen cyanide to give the 1,2,6-thiadiazine 2 . In the cyclocondensation reaction of 1 , with tetrachloromethane and phosphines Ph2PR′ (R′ = Ph2PNH or Ph) the 1,2,4,6,3,5-thiatriazaphosphorine 3 a , and the ring-open compound [t-BuS(NH)NHPPh3]Cl ( 4 ,), respectively, are formed by P? N-bond formation. The compounds are characterized by IR, MS and NMR data, and for 3a , further by X-ray structure analysis (space group P1 , Z = 2).  相似文献   

18.
Abstract

Infrared spectra of the coordination compounds [MG2(py)2], M(II)=Co, Ni, Cu and Zn; G=glycolato, py=pyridine, have been fully assigned by means of py and py-d 5 and glycolato α—OH and α—OD (G-d) labelling as well as metal ion substitution in the 4000–70cm?1 region. The crystal structure of the Ni(II) compound is presented and the spectra of the compounds are discussed on the basis of their structure and their bonding to the glycolato and pyridine ligands. Vibrational frequencies obtained for the Ni(II) compound are compared to those obtained by calculations carried out using the Gaussian 94 program package.  相似文献   

19.
A series of di‐nuclear ruthenium arene complexes with TSC ligands ([(η6p‐cymene)Ru(N1,S‐TSC)]2Cl2, A‐type, 1 and 2 ) and their corresponding analogues ([(η6p‐cymene)Ru(N2,S‐TSC)]2Cl2, B‐type, 3 and 4 ), in which TSCs act as different coordination mode, have been synthesized and structurally characterized by a variety of physical methods. The molecular structures of 1 , 3 and 4 were determined using single‐crystal X‐ray diffraction analysis. The Gibbs free energy of the two examples of the two types of complexes ( 1 and 3 ) and bonding order in their single‐crystals were discussed using density functional theory (DFT) calculations. The compounds were further evaluated for their in vitro antiproliferative activities against several cancerous and HEK‐293 T noncancerous cell lines, and the results indicate that B‐type complexes show stronger cytotoxicity than A‐type complexes. Furthermore, the interactions of the compounds with DNA were investigated by electrophoretic mobility spectrometry studies.  相似文献   

20.
Some new transition metal imidazolehydrogendicarboxylate hydrates of empirical formula M(Himdc)2·nH2O (H 2 imdc=4,5-imidazoledicarboxylic acid), where n=2 for M=Mn, Ni, Zn, Cd and n=3 for M=Co, have been prepared in aqueous solution. The compounds have been characterized by analytical, electronic and IR spectroscopic, thermal analysis and X-ray powder diffraction studies. Electronic spectroscopic data suggest that the Co and Ni compounds are of spin free (high spin) type with octahedral geometry. For these compounds, the IR bands in the region 1750-1710 cm-1 has been assigned to stretching vibrations of the non-ionized carboxylic group, confirming that the ligand is monoionized. IR spectra also suggest the unidentate co-ordination behaviour of carboxylate (vasy =1570 and vsym=1390 cm-1) groups of the imidazoledicarboxylate monoanion. The thermal behaviour of these compounds has been studied by simultaneous TG-DTA techniques. All of these compounds are dihydrates except cobalt which is a trihydrate. Thermal decomposition studies show that they lose two water molecules endothermally in the range 200-270°C to give their anhydrous compounds, indicating that these water molecules are coordinated to the metal. The anhydrous compounds further decompose exothermally in the range 300-620°C to leave the respective metal oxides via the metal oxalate intermediates. Whereas the manganese compound undergoes pyrolytic cleavage in a single step to give the manganese carbonate as the final residue. Isomorphic nature of these compounds is evident from XRD data. Six-coordination for the metal atoms has been proposed based on the thermal analysis, visible and IR spectroscopic results. This revised version was published online in August 2006 with corrections to the Cover Date.  相似文献   

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