Synthesis,crystal and molecular structure of 2-(3-chloropropyl)-6-methyl-4-phenylquinazoline 3-oxide

The acylation of the syn isomer of the oxime of 2-amino-5-methylbenzophenone with 4-chlorobutyryl chloride gives a mixture of the anti isomer of the 4-chlorobutyryloximine of 2-(4-chlorobutyryl)amino-5-methylbenzophenone and 2-(3-chloropropyl)-6-methyl-4-phenylquinazoline 3-oxide. The crystal and molecular structure of this oxide was established by X-ray diffraction structural analysis. The molecule is planar. The electron impact fragmentation of 2-(3-chloropropyl)-6-methyl-4-phenylquinazoline 3-oxide was discussed. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 1043–1051, July, 2007.     

Conventional radical polymerization and iodine‐transfer polymerization of 4′‐nonafluorobutyl styrene: Surface and thermal characterizations of the resulting poly(fluorostyrene)s

4′‐Nonafluorobutylstyrene (3) was synthesized and polymerized by conventional and controlled radical polymerization (iodine transfer polymerization (ITP)). Such an aromatic fluoromonomer was prepared from Ullmann coupling between 1‐iodoperfluorobutane and 4‐bromoacetophenone followed by a reduction and a dehydration in 50% overall yield. Two radical polymerizations of (3) were initiated by AIBN either under conventional or controlled conditions, with 1‐iodoperfluorohexane in 84% monomer conversion and in 50% yield. ITP of (3) featured a fast monomer conversion and a linear evolution of the ln([M]₀/[M]) versus time. The kinetics of radical homopolymerization of (3) enabled one to assess its square of the propagation rate to the termination rate (k_p²/k_t) in ITP conditions (36.2·10^?2 l·mol^?2·sec^?2 at 80 °C) from the Tobolsky's kinetic law. Polydispersity index (?) of the fluoropolymer achieved by conventional polymerization was 1.30 while it worthed 1.15 when synthesized by ITP. Thermal stabilities of these oligomers were satisfactory (10% weight loss under air occurred from 305 °C) whereas the melting point was 47 °C. Contact angles and surface energies assessed from spin‐coated poly(3) films obtained by conventional (hysteresis = 18°, surface energy 18 mN.m^?1) and ITP (hysteresis = 47°, surface energy 15 mN.m^?1) evidenced ? values' influence onto surface properties of the synthesized polymers. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 3202–3212     

Copoly(arylene phthalides) in the thermal polymerization of styrene

Russian Chemical Bulletin - The thermal polymerization of styrene in the presence of polymer initiators, copoly(arylene phthalides) of the diphenyl oxide series with different ratios of two...     

The thermal degradation of polysiloxanes—Part 4: Poly(dimethyl/diphenyl siloxane)

Poly(dimethyl/diphenyl siloxanes) have been prepared with a range of phenyl group contents both from mixtures of dimethyl and diphenyl cyclic siloxanes and from cyclic siloxanes in which both dimethyl and diphenyl structures are present. Attempts to prepare poly(diphenyl siloxane) with a reasonably high molecular weight were unsuccessful.The products of degradation of the poly(dimethyl/diphenyl siloxanes) are benzene and complex mixtures of cyclic oligomers which have been separated, identified and analysed. The characteristics of the formation of these products are discussed in relation to the degradation reactions which occur in poly(dimethyl siloxane), poly(methyphenyl siloxane) and poly(dimethyl/methylphenyl siloxane) and which have been described previously.     

Synthesis and Characterization of a Novel Ionic Liquid Polymer： Poly（1-（3-aminobenzyl）-3-methylimidazolium chloride）

A new type of polymerizable ionic liquid （IL） 1-（3-aminobenzyl）-3-methylimidazolium chloride （AMIC） was synthesized to obtain a novel polymer salt poly（1-（3-aminobenzyl）-3-methylimidazolium chloride） （PAMIC）. The AMIC was structurally characterized by mass spectrometry and Fourier transform infrared spectrometry （FTIR）. The structure, morphology and properties of PAMIC were investigated by FTIR, ultraviolet visible absorption spectra （UV-Vis）, scanning electron microscopy （SEM）, energy dispersive X-ray spectroscopy （EDX）, conductivity measurement and thermo- gravimetric analysis （TGA）. The PAMIC was spherulitic with an average diameter of about 50 nm and showed high conductivity and excellent thermal stability.     

Lithiation of 3-(Acylamino)-2-unsubstituted-, 3-(Acylamino)-2-ethyl-, and 3-(Acylamino)-2-propyl-4(3H)-quinazolinones: Convenient Syntheses of More Complex Quinazolinones(1)

3-(Pivaloylamino)- and 3-(acetylamino)-4(3H)-quinazolinones react with alkyllithium reagents to give 1,2-addition products in very good yields. Lithiation takes place with LDA and is regioselective at position 2. The lithium reagents thus obtained react with a variety of electrophiles to give the corresponding substituted derivatives in very good yields. Reactions of the lithium reagents with iodine give oxidatively dimerized cyclic structures. 3-(Pivaloylamino)- and 3-(acetylamino)-2-ethyl-4(3H)-quinazolinones and 3-(pivaloylamino)- and 3-(acetylamino)-2-propyl-4(3H)-quinazolinones are lithiated at the benzylic position with LDA. The lithium reagents so produced also react with a variety of electrophiles to give the corresponding 2-substituted-4(3H)-quinazolinone derivatives in very good yields. However, lithiation of 3-(acylamino)-2-(1-methylethyl)-4(3H)-quinazolinones was unsuccessful, as were lithiations of compounds having a diacetylamino group at position 3. The amide groups have been cleaved in good yield under basic or acidic conditions from some of the products to provide access to the free amino compounds.     

4-(4-溴丁基)苯乙烯的合成

4-(4-溴丁基)苯乙烯的合成;溴丁基苯乙烯;对氯苯乙酮;对氯苯乙烯;合成     

Syntheses,structures, and characterizations of two coordination polymers assembled from zinc(II) salts with 1,2-bis[3-(1,2,4-triazolyl)-4-amino-5-carboxylmethylthio]ethane

Two new coordination polymers, [ZnL] _n (1) and {[Zn(phen)(L)(H₂O)]?·?3H₂O} _n (2) (H₂L?=?1,2-bis[3-(1,2,4-triazolyl)-4-amino-5-carboxylmethylthio]ethane, phen?=?1,10-phenanthroline), have been synthesized and characterized by elemental analysis, IR, and X-ray diffraction. Polymer 1 is a 1-D infinite chain (space group P 1) and further forms a 3-D supramolecular structure by S?···?S interactions and hydrogen bonds. Polymer 2 displays a mononuclear structure (space group P 1) and extends into a 3-D supramolecular structure through hydrogen bonds. In addition, spectra and thermal stability of 1 and 2 are also discussed. Strong luminescence characteristics of both polymers are found, suggesting their potential applications as luminescent materials.     

(2R，3R)-和(2S，3S)-2-(4-羟基-3-甲氧基)-3-羟甲基-1，4-苯并二氧六环-6-醛的对映选择性合成

1,4-苯并二氧六环木脂素类天然产物多数具有增加胆碱乙酰化酶和抗肝毒等活性 ,其活性主要源于 1 ,4-苯并二氧六环官能团 [1] . 1 ,4-苯并二氧六环木脂素的消旋全合成已有报道 [2 ] ,但其不对称合成还是空白[3] .我们发展了一条对映选择性合成 1 ,4-苯并二氧六环木脂素的简捷有效的路线 .基于前面的工作 [4 ] ,我们发现 1 ,4-苯并二氧六环醛类衍生物是合成此类天然产物的关键中间体 ,选择 2 - (4-羟基- 3-甲氧基 ) - 3-羟甲基 - 1 ,4-苯并二氧六环 - 6-醛 (1 )作为目标分子 ,其合成路线如下 :Reagents and conditions:( ) Me OH,H2 SO4,9…     

Syntheses,characterizations, crystal structures,antibacterial and SOD-like activities of nickel(II) and copper(II) complexes with 2-((Z)-(4-methoxyphenylimino)methyl)-4,6-dichlorophenol

Three mononuclear nickel(II) and copper(II) complexes, [Ni(L)₂(py)₂] (1), [Ni(L)₂(DMF)(H₂O)] (2), and [Cu(L)₂] (3), where HL = 2-((Z)-(4-methoxyphenylimino)methyl)-4,6-dichlorophenol, py = pyridine and DMF = N,N-dimethylformamide, have been synthesized and their structures determined by single crystal X-ray analysis. Complexes 1–3 crystallized in the monoclinic system of the space groups C2/c, P2_1/n, and P2_1/c, respectively. The crystal structures of 1 and 2 present an octahedral geometry at the metal center and 3 shows a square-planar geometry. The FT-IR spectra, UV–vis spectra, and magnetic susceptibility measurements agree with the observed crystal structures. EPR spectra indicate a d_x2–y2 ground state (g_|| > g_⊥ > 2.0023 and A_|| > A_⊥) for 3 at RT and LNT. The results of simultaneous TG-DTA analyses of 1 and 3 showed the final degradation products are NiO for 1 and CuO for 3. The Schiff base (HL) behaves as monobasic bidentate ligand possessing N and O donor atoms. Electrochemical properties for the complexes are similar and involve two irreversible redox processes. Complex 3 exhibits the ability to inhibit jack bean urease, although its Schiff base has no ability to inhibit urease. Complex 1 exhibits more active scavenging effects against O₂^? than HL, 2 and 3 under the same conditions. Antibacterial screening activities of these complexes were also investigated.     

Syntheses, characterizations and crystal structures of triorganotin(IV) derivatives with 2-mercapto-4-quinazolinone

The triorganotin(IV) derivatives of 2-mercapto-4-quinazolinone (HSqualone) of the type, R₃SnL (R = Ph 1, CH₃2, PhCH₂3, p-F-PhCH₂4, o-F-PhCH₂5, n-Bu 6), were obtained by the reaction of the R₃SnCl and HSqualone with 1:1 molar ratio in benzene. All complexes 1-6 were characterized by elemental analyses, IR, ¹H and ¹³C NMR spectroscopy and the crystal structures of complexes 1-3 were also confirmed by X-ray crystallography. The structure analyses reveal that the tin atoms of complexes 1-3 are all distorted tetrahedral geometries. Furthermore, the dimeric structures in complexes 1-3 have also been found linked by intermolecular O-H?N or N-H?O hydrogen bonding interaction. Interestingly, the dimers of complexes 2 and 3 are further linked into one-dimensional chain through intermolecular C-H?S and C-H?O weak hydrogen bonding interactions, respectively.     

Phenolic products of radiation-thermal degradation of lignin as inhibitors for thermal polymerization of styrene

Fast 8-MeV electrons were used for the heating and dry distillation of hydrolytic lignin. The resulting tar differed in composition from that of the conventional dry distillation and was composed primarily of methoxyphenols. Guaiacol and creosol were the prevalent components in the fraction with the boiling range 80–235°C. It was shown that the tar effectively inhibits the thermal polymerization of styrene, with the inhibiting activity being higher than that of the commercial inhibitors Agidol 1 and Agidol 2. In the presence of 0.025 wt % tar, the induction period of the thermal polymerization of styrene at 120°C was at least 120 min.     

Syntheses of 1-, 2-, 3- and 4-acridinecarbaldehydes

The four acridinecarbaldehydes, namely, acridine-1-carbaldehyde, acridine-2-carbaldehyde, acridine-3-carbaldehyde, and acridine-4-carbaldehyde have been synthesized for the first time.     

Syntheses of 3-, 4-, and 5-O-feruloylquinic acids

The efficient synthesis of 3-, 4-, and 5-O-feruloylquinic acids starting from d-(?)-quinic acid is described. Esterification of suitably protected quinic acid derivatives with 3-(4-acetoxy-3-methoxyphenyl)-acryloyl chloride and subsequent hydrolysis of all the protecting groups afforded the title products in overall yields of 33%, 15%, and 45%, respectively, (from quinic acid).     

Syntheses, crystal structures and characterizations of two new quaternary thioborates: PbMBS4 (M = Sb, Bi)

Two new quaternary thioborates, PbSbBS(4) and PbBiBS(4), have been synthesized from solid-state reaction methods at temperatures from 1073 to 1123 K in evacuated sealed quartz tubes. The crystal structures have been determined by means of single crystal X-ray diffraction and they both crystallize in the P2(1)/m space group of the monoclinic system with a = 5.9532(18) ?, b = 6.2031(13) ?, c = 9.250(3) ?, β = 108.200(16)°, Z = 2 for PbSbBS(4) and a = 5.971(10) ?, b = 6.273(9) ?, c = 9.132(15) ?, β = 107.75(2)°, Z = 2 for PbBiBS(4), respectively. The two compounds are isostructural and both constructed with the infinite one-dimensional [MBS(4)](2-) (M = Sb or Bi) chains as building blocks, which are composed of [BS(3)](3-) trigonal plane units with [MS(3)](3-) (M = Sb or Bi) trigonal pyramids connected alternatively through corner-sharing along the crystallographic b axis. Two adjacent [MBS(4)](2-) chains are further bridged by the intermediate Pb(2+) cations, forming a novel S-shaped Pb-[MBS(4)] dimeric chain structure. In addition, first-principles electronic structure calculations based on the density functional theory (DFT) were performed on compound PbSbBS(4), indicating that the compound belongs to direct semiconductor with a band gap of 1.803 eV, which is in good agreement with the experimental value estimated from the UV-Vis diffuse reflectance spectroscopy.     

Syntheses,structural characteristics,and antimicrobial activities of new organotin(IV) 3-(4-bromophenyl)-2-ethylacrylates

New organotin(IV) carboxylates, [n-Bu₂SnL₂] (1), [Et₂SnL₂] (2), [Me₂SnL₂] (3), [n-Oct₂SnL₂] (4), [n-Bu₃SnL] _n (5), [Me₃SnL] _n (6), and [Ph₃SnL] _n (7), where L?=?3-(4-bromophenyl)-2-ethylacrylate, were synthesized and characterized by elemental analysis, FT-IR, and multinuclear NMR (¹H, ¹³C, and ¹¹⁹Sn). Spectroscopic studies confirm coordination of L to the organotin moiety via COO group. Single-crystal X-ray analysis reveals bridging mode of coordination in 6. Packing diagram established a supramolecular cage-like structure for 6 due to Sn–O interactions (3.287?Å). Subsequent antimicrobial activities proved them to be active biologically.