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An exceptionally productive and sustainable procedure is described in this paper to fabricate 1-(benzothiazolylamino) methyl-2-naphthols using a novel green nanocomposite of chitosan and diethylenetriamine-modified graphene oxide, supported methanesulfonic acid (Ch@GO-DETA.MSA.). For the synthesis of the nanocomposite, maleic anhydride was first attached to chitosan, and then, graphene oxide was modified by diethylenetriamine (GO@DETA). Subsequently, nanocomposite was prepared from the reaction of chitosan-g-maleic anhydride and GO@DETA. Finally, methane sulfonic acid was added to the nanocomposite to afford Ch@GO-DETA.MSA. Structural properties of the nanocomposite were explored through various techniques including X-ray diffraction (XRD), thermal gravimetric analysis (TGA), FTIR spectroscopy, scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS). 1-(Benzothiazolylamino) methyl-2-naphthols were efficiently prepared in high to excellent yields through a multicomponent reaction of 2-aminobenzothiazole, aryl aldehydes, and 2-naphthol using Ch@GO-DETA.MSA. nanocomposite under solvent-free conditions. The proposed protocol exhibited superiority over several published protocols due to its nontoxicity and eco-friendly, catalytic ability, short reaction times, generality, efficiency, solvent-free condition, and simple workup.

A novel nanosheet-structured material, namely graphene oxide anchored with sulfonic acid-functionalized glycerin (GO@Gl-SO3H), was prepared and characterized by FTIR, EDS, FESEM, TEM and XRD analyses. Afterward, its catalytic performance was examined for the synthesis of N,N′-alkylidene bisamides through the reaction of benzamide (2 eq.) and arylaldehydes (1 eq.) under solvent-free conditions. GO@Gl-SO3H was a highly effective catalyst for the reaction and afforded the products in high yields and short reaction times.

An adduct compound containing dinaphtosulfide macrocyclic diamide and silicotungstic acid was prepared and characterized by elemental analyses, IR, UV–VIS spectrophotometry and diffuse reflectance spectrometry. The stoichiometry and stability of adduct were studied by conductometry in nitrobenzene (NB) solvent. This is the first report of the interaction of crown ether containing sulfur heteroatom and heteropoly acid. The interaction of the adduct compound with Hg2+ was studied by spectrophotometric and pH-metric methods in NB solvent. The formation constant of the Hg2+-adduct complex was calculated from the computer fitting of the obtained data. The extraction of Hg2+ and Pb2+ was studied from aqueous solution using this adduct compound.

In this research work, we report the synthesis of macrocyclicdiamides from the reaction of diesters and aliphatic diamines in the presence of caesium carbonate. It has been demonstrated that among the carbonate of alkali metals (Li2CO3, Na2CO3, K2CO3 and CS2CO3), CS2CO3 appears to be the best catalyst for macrocyclization. Diesters with different substitution patterns on the aromatic ring reacted smoothly with diamines under optimal conditions, affording the corresponding macrocycles in high yields. Introducing a rigid group (e.g., sulfone) on the substrate led to somewhat decreased yield. Various substrates proved to be suitable for this macrocyclization reaction, especially, the flexible ones.

New polyamides containing pyridine thioethers were prepared under microwave irradiation and their solubility, thermal behavior, viscosity, and nanostructures were evaluated. These polyamides showed good solubility, viscosity, and high thermal stability. The sizes of polymer species were evaluated using their SEM images.

In this research work, dinaphthyl sulfide diester was prepared from the reaction of 1,1′-thiobis (2-hydroxy naphthalene) and methylchloroacetate. Its aza-macrocyclic derivative was synthesized from the reaction of dinaphthyl sulfide diester and diethylenetriamine. Lariats were prepared from the reaction of chloroamides (four derivatives) and initial macrocycle. Chloroamides were synthesized from the reaction of amines (aniline, benzylamine, 8-amino quinoline and 4-amino azobenzene) and chloroacetyl chloride. All the materials were identified by IR,1H NMR,13C NMR, and mass spectroscopies, and elemental analysis.

Some new aza thia crowns were prepared. A new diester was first prepared from the reaction of α,α′-bis(bromomethyl) benzene and methylthioglycolate. Aza crowns were synthesized from the reactions of this diester and diamines (ethylenediamine, 1,3-diaminopropane, 1,4-diaminobutane, 1,6-diaminohexane, and diethylenetriamine) in refluxing methanol (conventional heating) and under microwave (MW) irradiation. Based on the yields of aza crowns under these two conditions, MW irradiation is the better medium for these syntheses.

In this work, the efficiency, generality and applicability of novel Bronsted acidic ionic liquid triethylamine-bonded sulfonic acid {[Et 3 N–SO 3 H]Cl, N , N -diethyl- N -sulfoethanammonium chloride} as homogeneous and green catalyst for organic transformations under various conditions are studied. Herein, the following one-pot multi-component reactions in the presence of {[Et 3 N–SO 3 H]Cl are investigated: (i) the synthesis of β-acetamido ketones from acetophenones, aldehydes, acetonitrile and acetyl chloride in solution and under extremely mild conditions (room temperature), (ii) the preparation of 1,8-dioxo-octahydroxanthenes from dimedone (5,5-dimethyl-1,3-cyclohexanedione) (2 equiv.) and aldehydes (1 equiv.) under solvent-free conditions at moderate temperature (80 °C), and (iii) the synthesis of 14-aryl-14 H -dibenzo[ a,j ]xanthenes from β-naphthol (2 equiv.) and aldehydes (1 equiv.) in harsh conditions (120 °C) in the absence of solvent. High yields, relatively short reaction times, efficiency, generality, clean process, simple methodology, low cost, easy work-up, ease of preparation and regeneration of the catalyst and green conditions (in the synthesis of the xanthene derivatives) are advantages of the application of [Et 3 N–SO 3 H]Cl as catalyst in the above organic reactions. This work is the first report of the ionic liquid.

New dinaphthosulfoxide aza crowns were prepared from the corresponding dinaphthosulfoxide diester and diamines under reflux conditions (conventional heating) and microwave (MW) irradiation. These reaction routes were used for the synthesis of a series of aza crowns, such as dinaphthosulfide, dinaphthosulfone, dibenzosulfide, and dibenzosulfoxide. The synthesis of aza crowns under MW irradiation in comparison with conventional heating has several advantages, such as shorter reaction times, simpler reaction conditions, and the use of ecofriendly solvents, higher yields, and regioselectivity. In the MW synthesis, macrocyclization is preferred to oligomerization, and thus, the yields of byproducts are low. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. GRAPHICAL ABSTRACT

New dinaphthosulfide aza oxa thia crowns from 1-naphthol were prepared. At first, 2,2′-thiobis(1-hydroxynaphthalene) (a dinaphthol) was prepared from 1-naphthol. Then diester was prepared from the reaction of dinaphthol and methylchloroacetate. Aza crowns were synthesized from the reaction of diester and diamines (ethylene diamine, 1,3-diaminopropane, 1,4-diaminobutane, and 1,6-diaminohexane) in methanol. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. GRAPHICAL ABSTRACT

Dinaphthosulfone aza macrocycles were synthesized from the reaction of diamines and dinaphthosulfone diester (1,1′-sulfoxobis-(2-naphthoxy(2-methyl acetate))) in methanol in the presence of catalytic amounts of para toluenesulfonic acid (p-TsOH). Dinaphthosulfone diester (1,1′-sulfoxobis-(2-naphthoxy(2-methyl acetate))) was synthesized from the corresponding dinaphthosulfide diester and hydrogen peroxide in formic acid at room temperature. Dinaphthosulfide diester was prepared from initial dinaphtholsulfide diol (1,1′-thio bis(2-hydroxy naphthalene)) and methylchloroacetate. 1H NMR spectroscopy showed the unusual splittings for these dinaphthosulfone aza macrocycles, and this finding could be proposed as the role of tetrahedral structure of sulfone functional group, hydrogen bonding in the cavity and size of macrocycle.

Four new dinaphthosulfide and dibenzosulfide aza podands were synthesized. The synthesis of these podands was performed under three different reaction conditions: 1) diester, K 2 CO 3 , methanol, and RT; 2) diester, ethanolamine, and microwave (MW); and 3) diacid dichloride, ethanolamine, Et 3 N, CH 2 Cl 2 , RT. Two kinds of diester (dinaphthosulfide and dibenzosulfide) were used for the preparation of dihydroxy podands. These dihydroxy podands were reacted with thionyl chloride to afford dichloro podands. The second route gave excellent yields of dihydroxy podands. Dichloro podands are more soluble than dihydroxy podands in conventional solvents such as methanol, chloroform, and acetonitrile.

Some dinaphthosulfide aza macrocycles (3–9) were synthesized based on the conventional route from the reaction of corresponding dinaphthosulfide diester and aliphathic diamines in refluxing methanol in good yields. Dinaphthosulfide diester were synthesized from the reaction of 1,1′-thiobis (2-hydroxy naphthalene) and methyl chloroacetate. The structures of these compounds were confirmed using IR, 1H NMR, 13C NMR, MASS spectroscopy and elemental analysis. Conductometric studies of the complexation of some metal ions with aza derivative 8 (TDN) in methanol as solvent implied the formation of 1:1 complexes. The stability of the 1:1 complexes of TDN decreases in the order Hg2+ >> Pb2+ > Cu2+ > Zn2+ > Ca2+ > Mg2+ > Cd2+ > Sr2+ > Ag+ > Ba2+.

New dinaphthosulfide podands [3(a, b, and c)] were synthesized. The structures of these compounds were confirmed by IR, 1H NMR, 13C NMR, and Mass spectra. A simple, efficient, and sensitive procedure is described for the spectrophotometric determination of a trace amount of Ag+, Hg2+, Cr3+, Pb2+, and Ni2+ cations in the presence of Mn2+, Co2+, Cd2+ cations using the podand (3a). Formation constants of 1:1 complexes were determined from the absorbance-mole ratio data and found to vary in the order Pb2+ > Ni2+ > Hg2+ > Cr3+ > Ag+.

2,2′-Sulfinyl-bis(4-methyl phenol) 3 and it's thio derivative have been synthesized in this work. The reduction process of sulfoxide 3 to its thio derivative 5 was accomplished in the presence of Zn/AcOH/SiO2, under microwave irradiation. The structures have been confirmed by spectroscopic (IR, 1HNMR, 13CNMR) and single crystal x-ray diffraction methods. 2,2′-Sulfinyl-bis(4-methyl phenol) 3 crystallizes in the space group Cc of the monoclinic system with four molecules in the unit cell of dimensions a = 11.425(2) A, b = 13.530(2) A, c = 9.5215(17) A, β = 117.289(4) A, and 2,2′-thio-bis(4-methyl phenol) 5 crystallizes in the space group P 212121 of the orthorhombic system with four molecules in the unit cell of dimensions a = 9.021(1) A, b = 10.523(2) A, c = 13.607(2) A, α = 90. The structures have been refined to final values for the crystallographic R factor of 0.0189(3) and 0.0248(5) based on 2999 and 3720 observed independent reflections respectively.

We report the synthesis of new polyamides containing 2,6-bis(2-thio-2-(4-carboxyphenyl)-1-oxo)pyridine subunit, under microwave irradiation using Yamasaki phosphorylation method. The solubility, thermal behavior, and viscosity of polyamides were evaluated. The structures of polymers have been characterized using IR and 1H NMR spectroscopy. These polyamides showed good solubility, viscosity, high thermal stability, and glass transition temperatures. Their viscosities and glass transition temperatures are in the range of 0.63–0.88 and 223–295°C, respectively. Thermal stabilities for 10% weight loss (T10) are 137–173°C and for 50% weight loss (T50) are in the range of 483–523°C. The study of surface morphology showed particle and amorphous structures.

New aza thia crowns were prepared from the reaction of 2,2′-diaminodiphenyl disulfide and diacids or diacid chlorides. Diacids are malonic acid, adipic acid, sebacic acid, and 2,2′-thiodiacetic acid and diacid dichlorides are malonyl chloride, adipoyl chloride, sebacoyl chloride, and 2,2′-thiodiacetyl chloride. [Supplementary materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfer, and Silicon and the Related Elements for the following free supplemental files: Additional figures.]

A highly efficient, green and simple solvent-free method for the synthesis of 1-amidoalkyl-2-naphtholsviaone-pot multi-components condensation of 2-naphthol, aromatic aldehydes and amides in the presence of catalytic amount of silica-supported molybdatophosphoric acid (H3PMo12O40.xH2O/SiO2, 3.17 mol%) is described. The reactions proceed rapidly and the title compounds are produced in high to excellent yields.