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1.
The 1‐aroyl‐1‐aryl‐2‐bromocyclopentanes 3a , 3b , 3c and 3d (Ar = C6H5, 2‐FC6H4, 3‐FC6H4, 4‐FC6H4) were prepared from N‐bromosuccinimide (NBS)‐promoted rearrangement of 1,1‐diarylmethylenecyclopentane 2 . The possible mechanism was proposed. Two 1‐phenyl‐cyclopentane carbamides 5a and 5b with the anti‐influenza effect were also accomplished from compound 3a .  相似文献   

2.
4‐(5‐oxo‐1,2,4‐triazol‐3‐yl)‐sydnones 11 and 4‐(4‐arylamino‐5‐oxo‐1,2,4‐triazol‐3‐yl)‐sydnones 13 have been obtained from a‐chloroformylarylhydrazine hydrochloride 2 . Moreover, the intermediates, including 3, 4 , 9 and 10 , in this study are synthetically informative and valuable. It is also noteworthy that three reactants, 1, 2 and sydnonecarbaldehydes, were prepared from sydnone derivatives and their fragments. The oxidative cyclizations of sydnonecarbaldehyde semicarbazones 9 and carbazones 10 with two different oxidizing agents (Cu(ClO4)2 and Fe(ClO4)3) have been extensively examined. The reaction time and the yields of cyclizations were affected by the substituents of semicarbazones 9 and carbazones 10.  相似文献   

3.
An SO3H‐functionalized nano‐MGO‐D‐NH2 catalyst has been prepared by multi‐functionalization of a magnetic graphene oxide (GO) nanohybrid and evaluated in the synthesis of tetrahydrobenzo[b]pyran and pyrano[2,3‐d]pyrimidinone derivatives. The GO/Fe3O4 (MGO) hybrid was prepared via an improved Hummers method followed by the covalent attachment of 1,4‐butanesultone with the amino group of the as‐prepared polyamidoamine‐functionalized MGO (MGO‐D‐NH2) to give double‐functionalized magnetic nanoparticles as the catalyst. The prepared nanoparticles were characterized to confirm their synthesis and to precisely determine their physicochemical properties. In summary, the prepared catalyst showed marked recyclability and catalytic performance in terms of reaction time and yield of products. The results of this study are hoped to aid the development of a new class of heterogeneous catalysts to show high performance and as excellent candidates for industrial applications.  相似文献   

4.
A nanostructured organic–inorganic framework, hexagonal NH2‐MIL‐88B, has been prepared through a facile one‐pot reflux reaction and then it was characterized using various techniques. The as‐prepared sample with high specific surface area (414 m2 g?1) showed excellent adsorption for 2,4,6‐trinitrophenol (TNP) in the liquid phase. Detailed studies of the adsorption kinetics, adsorption mechanism, adsorption isotherm, activation energy and various thermodynamic parameters were conducted. The adsorption mechanism of NH2‐MIL‐88B for TNP may be ascribed to hydrogen bond interaction, and the complexation between ─OH in TNP and unsaturated Fe(III) on the surface of NH2‐MIL‐88B. The maximum adsorption capacity of NH2‐MIL‐88B for TNP based on the Langmuir isotherm was 163.66 mg g?1. The as‐prepared NH2‐MIL‐88B adsorbent seems to be a promising material in practice for TNP removal from aqueous solution.  相似文献   

5.
David M. Casper 《合成通讯》2013,43(20):3501-3507
N‐tert‐Butyldecahydro‐3‐isoquinoline carboxamide (1) is a key structural fragment present in a variety of medicinally important HIV protease inhibitors. Derivatives of this carboxamide were prepared by alkylation with either 2‐iodoethanol, allyl bromide, or bromoacetaldehyde dimethylacetal. The corresponding aldehyde of the dimethylacetal derivative was prepared by reaction with BBr3 in CH2Cl2.  相似文献   

6.
Propene (P)/4‐methyl‐1‐pentene (Y) copolymers in a wide range of composition were prepared with isospecific single center catalysts, rac‐Et(IndH4)2ZrCl2 ( EBTHI ), rac‐Me2Si(2‐Me‐BenzInd)2ZrCl2 ( MBI ), and rac‐CH2(3‐tBuInd)2ZrCl2 ( TBI ). 13C NMR analysis of copolymers and statistical elaboration of microstructural data at triad level were performed. Unprecedented and surprising results are here reported. Random P/Y copolymers were prepared with the most isospecific catalyst, TBI , that is known to prepare ethene/propene and ethene/4‐methyl‐1‐pentene copolymers with long homosequences of both comonomers, whereas longer homosequences of both comonomers were observed in copolymers from the less enantioselective metallocenes EBTHI and MBI . These findings, which are against what is acknowledged in the field, can pave the way for the preparation on a large scale of random propene‐based copolymers. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2015 , 53, 2575–2585  相似文献   

7.
A new approach to obtain imide‐containing elastic polymers (IEPs) via elastic and high‐molecular‐weight polyureas, which were prepared from α‐(4‐aminobenzoyl)‐ω‐[(4‐aminobenzoyl)oxy]‐poly(oxytetramethylene) and the conventional diisocyanates such as tolylene‐2,4‐diisocyanate(2,4‐TDI), tolylene‐2,6‐diisocyanate(2,6‐TDI), and 4,4′‐diphenylmethanediisocyanate (MDI), was investigated. IEP solutions were prepared in high yield by the reaction of the polyureas with pyromellitic dianhydride in N‐methyl‐2‐pyrrolidone (NMP) at 165°C for 3.7–5.2 h. IEPs were obtained by the thermal treatment at 200°C for 4 h in vacuo after NMP was evaporated from the resulting IEP solutions. We assumed a mechanism of the reaction via N‐acylurea from the identification of imide linkage and amid acid group in IEP solutions. NMR and FTIR analyses confirmed that IEPs were segmented polymers composed of imide hard segment and poly(tetramethylene oxide) (PTMO) soft segment. The dynamic mechanical and thermal analyses indicated that the IEPs prepared from 2,6‐TDI and MDI showed a glass‐transition temperature (Tg ) at about −60°C, corresponding to Tg of PTMO segment, and suggested that microphase‐separation between the imide segment and the PTMO segment occured in them. TGA studies indicated the 10% weight‐loss temperatures (T10) under air for IEPs were in the temperature range of 343–374°C. IEPs prepared from 2,6‐TDI and MDI showed excellent tensile properties and good solvent resistance. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 715–723, 2000  相似文献   

8.
2,3‐Dihydro‐4H‐thiopyrano[2,3‐b]pyridin‐4‐ones 4 were prepared by a three‐step sequence from commercially available 2‐chloropyridine ( 1 ). Thus, successive treatment of 1 with iPr2NLi (LDA) and α,β‐unsaturated aldehydes gave 1‐(2‐chloropyridin‐3‐yl)alk‐2‐en‐1‐ols 2 , which were oxidized with MnO2 to 1‐(2‐chloropyridin‐3‐yl)alk‐2‐en‐1‐ones 3 . The reactions of 3 with NaSH?n H2O proceeded smoothly at 0° in DMF to provide the desired thiopyranopyridinones. Similarly, 2,3‐dihydro‐4H‐thiopyrano[2,3‐c]pyridin‐4‐ones 8 and 2,3‐dihydro‐4H‐thiopyrano[3,2‐c]pyridin‐4‐ones 12 were obtained starting from 3‐chloropyridine ( 5 ) and 4‐chloropyridine ( 9 ), respectively.  相似文献   

9.
1,1‐Bis[4‐(4‐aminophenoxy)phenyl]‐1‐phenylethane (BAPPE) was prepared through nucleophilic substitution reaction of 1,1‐bis(4‐hydroxyphenyl)‐1‐phenylethane and p‐chloronitrobenzene in the presence of K2CO3 in N,N‐dimethylformamide, followed by catalytic reduction with hydrazine and Pd/C. Novel organosoluble polyimides and copolyimides were synthesized from BAPPE and six kinds of commercial dianhydrides, including pyromellitic dianhydride (PMDA, Ia ), 3,3′,4,4′‐benzophenonetetracarboxylic dianhydride (BTDA, Ib ), 3,3′,4,4′‐ biphenyltetracarboxylic dianhydride (BPDA, Ic ), 4,4′‐oxydiphthalic anhydride (ODPA, Id ), 3,3′,4,4′‐diphenylsulfonetetracarboxylic dianhydride (DSDA, Ie ) and 4,4′‐hexafluoroisopropylidenediphthalic anhydride (6FDA, If ). Differing with the conventional polyimide process by thermal cyclodehydration of poly(amic acid), when polyimides were prepared by chemical cyclodehydration with N‐methyl‐2‐pyrrolidone as used solvent, resulted polymers showed good solubility. Additional, Ia,b were mixed respectively with the rest of dianhydrides (Ic–f) and BAPPE at certain molar ratios to prepare copolyimides with arbitrary solubilities. These polyimides and copolyimides were characterized by good mechanical properties together with good thermal stability. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 2082–2090, 2000  相似文献   

10.
The palladium(II) and platin(II) 1, 1‐dicyanoethylene‐2, 2‐dithiolates [(L–L)M{S2C=C(CN)2}] (M = Pd: L–L = dppm, dppe, dcpe, dpmb; M = Pt: dppe, dcpe, dpmb) were prepared either from[(L–L)MCl2] and K2[S2C=C(CN)2] or from [(PPh3)2M{S2C=C(CN)2}] and the bisphosphane. Moreover, [(dppe)Pt{S2C=C(CN)2}]was obtained from [(1, 5‐C8H12)Pt{S2C=C(CN)2}] and dppeby ligand exchange. The 1, 1‐dicyanoethylene‐2, 2‐diselenolates[(dppe)M{Se2C=C(CN)2}] (M = Pd, Pt) were prepared from[(dppe)MCl2] and K2[Se2C=C(CN)2]. The oxidation potentials of the square‐planar palladium and platinum complexes were determined by cyclic voltammetry. The reaction of [(dcpe)Pd(S2C=O)] with TCNE led to a ligand fragment exchange and gave the 1, 1‐dicyanoethylene‐2, 2‐dithiolate [(dcpe)Pd{S2C=C(CN)2}] in good yield.  相似文献   

11.
A CF3‐containing diamine, 1,4‐bis(4‐amino‐2‐trifluromethylphenoxy) benzene ( I ), was prepared from hydroquinone and 2‐chloro‐5‐nitrobenzotrifluoride. Imide‐containing diacids ( V a–h and VI a,b ) were prepared through the condensation reaction of amino acids, aromatic diamines, and trimellitic anhydride. Then, a series of soluble fluorinated polyamides ( VII a–h ) and poly(amide imide)s ( VIII a–h and X a,b ) were synthesized from I with various aromatic diacids ( II a–h ) and imide‐containing diacids ( V a–h and VI a,b ) via direct polycondensation with triphenyl phosphate and pyridine. The polyamides and poly(amide imide)s had inherent viscosities of 1.00–1.70 and 0.79–1.34 dL/g, respectively. All the synthesized polymers showed excellent solubility in amide‐type solvents such as N‐methyl‐2‐pyrrolidinone, N,N‐dimethylacetamide, and N‐dimethylformamide and afforded transparent and tough films via solvent casting. Polymer films of VII a–h , VIII a–h , and X a,b had tensile strengths of 91–113 MPa, elongations to break of 8–40%, and initial moduli of 2.1–2.8 GPa. The glass‐transition temperatures of the polyamides and poly(amide imide)s were 254–276 and 255–292 °C, respectively, and the imide‐containing poly(amide imide)s had better thermal stability than the polyamides. The polyamides showed higher transparency and were much lighter in color than the poly(amide imide)s, and their cutoff wave numbers were below 400 nm. In comparison with isomeric IX c – h , poly(amide imide)s VIII c–h exhibited less coloring and showed lower yellowness indices. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 3116–3129, 2004  相似文献   

12.
The surface of Fe3O4 magnetic nanoparticles (MNPs) was modified by chloropropylsilane and histidine. The imidazole group of prepared Fe3O4@Propylsilane@Histidine MNPs converted to imidazolium hydrogen sulfate group and Fe3O4@Propylsilane@Histidine [HSO4] as a novel environmentally friendly ionic liquid/ magnetite nanoparticle was prepared, successfully. FT‐IR, XRD, SEM and TEM instruments was used to identifiy the histidine ionic liquids/magnetite nanoparticles (HILMNPs). The catalytic activity of synthesized HILMNPs was appraised for the synthesis of 9‐aryl‐1,8‐dioxooctahydroxanthene and spiro[indoline‐3,9′‐xanthene]trione derivatives. The activity of HILMNPs was much better than the other reported heterogeneous and homogeneous catalysts. Furthermore, the prepared catalyst could be separated from the reaction mixture and reused four times without any significant loss in its activity.  相似文献   

13.
《合成通讯》2013,43(12):2269-2275
Abstract

Mild and efficient procedures have been developed for synthesis of 1,8‐naphthalide and 1,8‐naphthalenedimethanol. In an ice‐water bath, 1,8‐naphthalide was prepared from 1,8‐naphthlic anhydride using LiAlH4 as reducing agent. 1,8‐Naphthalenedimethanol was obtained with good yield from reduction of 1,8‐naphthalic anhydride by LiAlH4 and Lewis acids at room temperature. The effects of various factors on the reduction of 1,8‐naphthalic anhydride with LiAlH4 were investigated.  相似文献   

14.
The K‐V‐alkaline‐earth metal catalysts supported on α‐alumina ceramic substrate have been prepared. The morphology of the soot particulates deposited on prepared catalysts supported on α‐alumina ceramic substrate was described by scanning electron microscopy (SEM). The XRD was used to characterize the catalysts and their catalytic activities were evaluated by soot oxidation reaction using the TPR system. The SEM photographs presented that soot particles have a particle size of about 100 nm in diameter forming a loose contact with catalyst, which is resemble to the real situation for the catalyst application. The XRD and TPR study showed that the catalytic activities of the catalysts were improved through the cooperation of KNO3 and some alkaline earth metal compounds. The soot onset ignition temperature at 310°C is the lowest by the cooperation of the crystalline phases KNO3, KCaVO4, and Ca3(VO4)2 for the K‐V‐Ca catalyst with a molar ratio of 6:1:1. In addition, the catalyst containing higher KNO3 content has an adsorption for CO2. The all prepared K‐V‐Ba catalysts can adsorb more CO2 at room temperature.  相似文献   

15.
In this study, MnFe2O4 nanoclusters were prepared as bioprobes to establish a lateral‐flow immunochromatographic assay (LFIA) for the rapid and quantitative detection of D‐dimer for the first time. The magnetic properties of the magnetic labels play a key role in the quantitative detection of biomolecules. The 47.3‐nm MnFe2O4 magnetic nanoclusters (MNCs) with good dispersion and high saturation magnetization (76 emu/g) were fabricated via thermal decomposition of Fe(acac)3 with Mn(acac)2. The prepared MnFe2O4 MNCs were well dispersed in water because the surfaces were fully covered with 3,4‐dihydroxyhydrocinnamic acid (DHCA) molecules by ligand exchange. Anti‐D‐dimer antibodies were coupled on the surface of MnFe2O4 MNCs, and the target protein, D‐dimer, was detected, in the range 0.05–6 μg/mL. This assay provides a promising platform for D‐dimer detection for point‐of‐care diagnosis.  相似文献   

16.
A two‐step synthesis of 1‐substituted 3‐alkoxy‐1H‐isoindoles 4 has been developed. Thus, the reaction of 2‐(dialkoxymethyl)phenyllithium compounds, which are easily generated in situ by Br/Li exchange between 1‐bromo‐2‐(dialkoxymethyl)benzenes 1 and BuLi in THF at ?78°, with nitriles afforded [2‐(dialkoxymethyl)phenyl]methanimines 2 , which were treated with a catalytic amount of TsOH?H2O in refluxing CHCl3 to give the desired products in reasonable yields. Similarly, 3‐aryl‐1‐ethoxy‐1‐methyl‐1H‐isoindoles 7 have been prepared starting from 1‐bromo‐2‐(1,1‐diethoxyethyl)benzenes 5 .  相似文献   

17.
K. C. Majumdar  N. Kundu 《合成通讯》2013,43(10):1747-1756
A number of hitherto unreported 2H‐benzothiopyrano[3,2‐c]quinolin‐7(8H)‐ones have been regioselectively synthesized in 90–96% yield by tri‐n‐butyltinhydride–AIBN–mediated radical cyclization from 4‐(2′‐bromothioarylmethyl)‐1‐methylquinolin‐2(1H)‐ones and their corresponding sulfones. 4‐(2′‐Bromothioarylmethyl)quinolin‐2(1H)‐ones were in turn prepared from 4‐bromomethylquinolin‐2(1H)‐one and o‐bromothiophenols by refluxing in acetone in the presence of anhydrous K2CO3. These were converted to the corresponding sulfones by oxidation with two equivalents of m‐CPBA in refluxing dichloromethane for 1 h.  相似文献   

18.
2,3‐Dimethylpentacene (DMP) and 2,3‐dimethyltetracene (DMT) were synthesized, characterized and employed as the channel material in the fabrication of thin‐film transistors. The two methyl groups increase the chemical stability of the compounds versus the pristine acene analogues. The crystals maintain herringbone‐like molecular packing, whereas the weak dipole associated with the unsymmetrical molecule induces an anti‐parallel alignment among the neighbors. This structural motif favors layered film growth on SiO2/Si surface. Thin film transistors prepared on SiO2/Si and n‐nonyltrichlorosilane‐modified SiO2/Si at different substrate temperatures were compared. DMP‐based transistors prepared on rubbed n‐nonyltrichlorosilane‐modified SiO2/Si substrate gave the highest field‐effect mobility of 0.46 cm2/Vs, whereas DMT‐based transistor gave a mobility of 0.028 cm2/Vs.  相似文献   

19.
An aziridinomitosene skeleton, a basic core of mitomycin antibiotics, was straightforwardly prepared from N‐(p‐toluenesulfonyl)indole‐2‐carboxaldehyde in 16% overall yield by successive reactions of guanidinium ylide‐mediated aziridination, InCl3‐catalyzed epimerization of trans‐3‐(indol‐2‐yl)aziridine‐2‐carboxylate, leading to the cis‐derivative, and dehydrative cyclization.  相似文献   

20.
When a single metal fails to promote an efficient Suzuki‐Miyaura coupling reaction at ambient temperature, the synergistic cooperation of two distinct metals might improve the reaction. To examine the synergistic effect of palladium and nickel for catalyzing Suzuki coupling reaction, g‐C3N4 supported metal nanoparticles of PdO, NiO and Pd‐PdO‐NiO were prepared, characterized and their catalytic activities evaluated over different aryl halides at room temperature and 78 °C. The morphological characterization of Pd‐PdO‐NiO/g‐C3N4 demonstrated that the bimetallic particles were uniformly dispersed over the g‐C3N4 layers with diameters ranging from 3.5‐7.7 nm. XPS analysis showed that nanoparticles of Pd‐PdO‐NiO consisted of Pd(II), Pd(0) and Ni(II) sites. The experiments performed on the catalytic activity of Pd‐PdO‐NiO/g‐C3N4 showed that the prepared catalyst demonstrated an efficient activity without using toxic solvents.  相似文献   

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