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91.
A novel synthesis of thioxo-quinazolino[3,4-a]quinazolinone framework was developed through a four-step reaction starting from isatoic anhydride. The resulting 2-aminobenzamides from the reaction of isatoic anhydride and different amines underwent coupling–cyclization reaction with 2-nitrobenzaldehydes, reduction of nitro group, and then cyclization reaction with carbon disulfide (CS2). All steps were carried out under easy and user-friendly conditions in a short time without using expensive catalysts or reagents.
[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource(s): Full experimental and spectral details.] 相似文献
92.
Zerong Daniel Wang Meagan Hysmith Motoko Yoshida Ben George Perla Cristina Quintana 《International journal of quantum chemistry》2014,114(6):429-435
A benchmark comparison for different computational methods and basis sets has been presented. In this study, five computational methods (Hartree–Fock (HF), MP2, B3LYP, MPW1MP91, and PBE1PBE) along with 18 basis sets have been applied to optimize the geometry of carbon disulfide (CS2), and further calculate the vibrational frequencies of the optimized geometries. The differences between the calculated frequencies and corresponding experimental data are used to evaluate the efficiency of each combination of computational method and basis set. The comparison of frequency difference indicates that B3LYP generally gives the best prediction of frequencies for CS2, whereas the other two density functional theory (DFT) methods, i.e., MPW1PW91 and PBE1PBE, often give parallel results. Although MP2 predicts the frequencies with accuracy almost as good as those from DFT methods, in a particular case, HF calculation outperforms MP2 as well as MPW1PW91 and PBE1PBE for prediction of the frequency of asymmetrical stretching for CS2. © 2013 Wiley Periodicals, Inc. 相似文献
93.
采用N,N-二甲基甲酰胺(DMF)和四氢呋喃(THF)为溶剂,用离散法制备二硫化钼(MoS2)悬浮溶液,并用开孔Z扫描方法研究其在可见和近红外区域的非线性光学特性.结果显示,在强激光照射下,MoS2(in THF)悬浮溶液在可见波段(530 nm)透过率增强为常光透过率的1.54倍,表现为饱和吸收;在近红外波段(790 nm)透过率减弱为常光透过率的0.6倍,表现为反饱和吸收,具有很好的波长选择性光限幅效应.而作为对比的MoS2(in DMF)悬浮溶液在全波段透过率降低,呈现反饱和吸收特性,波长选择性不明显.机理解释可能为饱和吸收和热效应导致的自衍射两种机制联合作用. 相似文献
94.
Improved reaction conditions for the preparation of poly(p‐phenylene sulfide) (PPS) directly from bis(4‐bromophenyl) disulfide (BBD) have been established. Heating BBD with magnesium metal afforded only a low molecular weight polymer. PPS with a melting temperature around 280 °C was obtained from BBD in the presence of sodium carbonate or zinc metal. The best results were obtained with the addition of a catalytic amount of KI to the zinc–BBD mixture. Polymers prepared by the above methods are semicrystalline and dissolve in 1‐chloronaphthalene and have properties comparable to commercial PPS. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 900–904, 2006 相似文献
95.
Akane Suzuki Daisuke Nagai Bungo Ochiai Takeshi Endo 《Journal of polymer science. Part A, Polymer chemistry》2004,42(23):5983-5989
The trifunctional five‐membered cyclic carbonate 2 and dithiocarbonate 3 were successfully synthesized by the reaction of trifunctional epoxide 1 with carbon dioxide and carbon disulfide, respectively. The crosslinking reactions of 2 with p‐xylylenediamine or hexamethylenediamine were carried out in dimethyl sulfoxide at 100 °C for 48 h to produce the corresponding crosslinked poly(hydroxyurethane)s quantitatively. The crosslinking reactions of 3 with both p‐xylylenediamine and hexamethylenediamine, followed by acetylation of thiol moiety, produced the corresponding crosslinked poly(thioester–thiourethane)s quantitatively. The obtained crosslinked poly(hydroxyurethane)s were thermally more stable than the analogous crosslinked poly(thioester–thiourethane)s, probably because of less thermal stability of thiourethane moiety than hydroxyurethane moiety. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 5983–5989, 2004 相似文献
96.
97.
Twelve-membered ring pseudopeptidic cyclic disulfides have been prepared by iodine oxidation of the parent dithiols. However, oxidation of N,N′-(1,2-phenylene)bis(2-mercapto-2-methylpropanamide) afforded a 25/75 mixture of cyclic mono- and bis-disulfides that were separated by selective precipitation in CHCl3. The cyclic bis-disulfide was selectively prepared by iodine oxidation of the Ni complex of this dithiol and crystallized. Its crystal structure was solved by X-ray diffraction. All these cyclic mono- or bis-disulfides were selectively converted to cyclic mono- and bis-thiosulfinates upon stoichiometric oxidation with dimethyldioxirane at low temperature. 1H NMR of the cyclic bis-thiosulfinate revealed the presence of four isomers, two couples of stereoisomers, as expected from the insertion of two oxygen atoms in this compound, one on each disulfide bond. The two couples of cis/trans isomers were separated by preparative TLC and identified after alkaline cleavage of the two S(O)-S bonds and metalation with Ni(II). As HO− attack is selective for the sulfinyl sulfur, the nature of the Ni complexes obtained is a signature of each couple of stereoisomers. 相似文献
98.
Wenjian Xu Xiulin Zhu Zhenping Cheng Gaojian Chen Jian Zhu 《Journal of polymer science. Part A, Polymer chemistry》2005,43(3):543-551
The bulk polymerization of styrene was investigated with tetramethylthiuram disulfide (TMTD) as an initiator in the presence of 2,2,6,6‐tetramethyl‐1‐piperidinyloxy (TEMPO) at 123 °C. The polymerization proceeded in a controlled/living way; that is, the polymerization rate was first‐order with respect to the monomer concentration, and the molecular weight increased linearly with conversion. The molecular weights of the polymers obtained were close to the theoretical values, and the molecular weight distributions were relatively low (weight‐average molecular weight/number‐average molecular weight = 1.1–1.3). The rate of polymerization with TMTD as an initiator was faster than that with benzoyl peroxide, and the rate was independent of the initial concentration of TMTD in the presence of TEMPO. The obtained polystyrene was functionalized with ultraviolet‐light‐sensitive ? SC(S)N(CH3)2 groups, which was characterized with 1H NMR spectroscopy. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 543–551, 2005 相似文献
99.
《Magnetic resonance in chemistry : MRC》2003,41(1):37-41
The oxidation of symmetrical disulfides [D ,L ‐cystine ( 1 ) and 3,3′‐dithiobis(propionic acid) ( 2 )] with hydrogen peroxide in D2O–NaOH solution (pH 10–11) was studied by NMR spectroscopy. Assignments of the proton and carbon NMR signals of starting materials ( 1 and 2 ) and products of oxidation are based on conventional 1D NMR methods (DEPT, selective spin decoupling). Formation of C—S bond cleavage products or, in case of 2 , partially oxidized intermediates was not detected. The accelerating effect of Cu2+ cations, but not Fe3+ cations, on the oxidation rate of 1 in basic medium was demonstrated. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
100.
《Magnetic resonance in chemistry : MRC》2003,41(8):585-588
A novel, radical responsive MRI contrast agent based on a gadolinium chelate conjugated to a liposome through a disulfide linker was synthesized, with the aim of pursuing the in vivo mapping of radicals. The liposome was prepared by incorporating a thiol‐activated phospholipid, which was subsequently reacted with a gadolinium chelate containing a free thiol group. The long reorientational motion of the supramolecular adduct endows the paramagnetic agent with a relaxivity significantly higher than that of the free complex. The disulfide bond represents a radical‐sensitive moiety and a large decrease in contrast efficacy (T1 relaxivity) is shown upon its cleavage. A preliminary assessment of the system was made by means of in vitro gamma‐irradiation and thiol–disulfide bond exchange with dithiothreitol. Both methods showed a clear dose‐dependent decrease in T1‐relaxivity. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献